CN105576211A - Method for preparing nitrogen-doped carbon-coated graphene material of lithium ion battery - Google Patents
Method for preparing nitrogen-doped carbon-coated graphene material of lithium ion battery Download PDFInfo
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- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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Abstract
The invention provides a method for preparing a nitrogen-doped carbon-coated graphene material of a lithium ion battery. The method is characterized by comprising the following steps: a, preparing graphene oxide suspension: preparing graphite oxide by adopting a hummer method, and ultrasonically peeling graphite oxide in deionized water to form graphene oxide suspension; and b, preparing the nitrogen-doped carbon-coated graphene material: adding a certain amount of cyanamide aqueous solution into the graphene oxide suspension, uniformly stirring, putting in a closed reaction kettle to perform hydrothermal reaction, washing a hydrothermal reaction product by using deionized water, drying, and processing at high temperature under the protective atmosphere so as to obtain the nitrogen-doped carbon-coated graphene material of the lithium ion battery. The method is simple, high in operability and good in repeatability.
Description
Technical field
The invention belongs to electrochemical material field, be specifically related to a kind of preparation method of lithium ion battery nitrogen-doped carbon coated graphite alkene material.
Background technology
Lithium ion battery has been widely used in portable equipment, as mobile phone, panel computer, laptop computer, camera etc.They propose new requirement to lithium ion battery: high magnification, high power capacity, safety and stability, longer useful life, technology maturation, low price, environmental friendliness etc.Facing to the requirement that these are new, lithium ion battery will be faced with various significant challenge, can adapt to this neozoic market fast.
Graphene is a kind of Novel Carbon Nanomaterials, becomes study hotspot now.Graphene is that basic structural unit is stable benzene hexatomic ring by a kind of carbonaceous new material of individual layer sp2 carbon atom tightly packed one-tenth bi-dimensional cellular shape lattice structure.This special microstructure, makes Graphene have larger theoretical specific surface area, causes and makes it have higher storage lithium ability.But, single grapheme material is used as electrode material, be subject to the restriction of factors, as excessive in Graphene specific surface, easily reunite between lamella, substantially increase irreversible capacity loss (lower initial coulomb efficiency (<73%)) and reduce it as electrode material conductivity, thus bringing harmful effect to electrode tablet making technology aspect.Particularly, single Graphene electric material is when high rate charge-discharge, and capacity attenuation is too fast.
Carbon coated core-shell nanostructure has been widely used in the electrode material of LIBs, and these nucleocapsid structures with carbohydrate as carbon source, can be able to be obtained by hydro thermal method one step.The excellent properties of core/shell material is relevant to their unique structures, the performance of nuclear particle is along with the improvement that is changed significantly of the shell be coated on around nuclear particle, this is the characteristic utilizing the cooperative effect of core/shell material and both interactions can produce multi-efficiency, overcomes defects most separately and the advantage of both performances.So, adopt the present invention's hydro-thermal used doping nitrogen method to prepare nitrogen-doped carbon coated graphite alkene material lithium ion battery negative material and there is outstanding chemical property.
Summary of the invention
The object of the invention is the doubly forthright difference for Graphene negative material, provide the preparation method of a kind of high power capacity, powerful nitrogen-doped carbon coated graphite alkene material, the method is simple, workable, reproducible.
For realizing above object of the present invention, the invention provides following technical scheme:
A preparation method for lithium ion battery nitrogen-doped carbon coated graphite alkene material, is characterized in that comprising the following steps:
A, preparation graphene oxide suspension: adopt hummer legal system for graphite oxide, by graphite oxide ultrasonic strip off formation graphene oxide suspension in deionized water;
B, prepare nitrogen-doped carbon coated graphite alkene material: in graphene oxide suspension, add a certain amount of cyanamide aqueous solution; stir; put into closed reactor and carry out hydro-thermal reaction; hydro-thermal reaction product is spent deionized water; dry; high-temperature process under protective atmosphere, obtains lithium ion battery nitrogen-doped carbon coated graphite alkene material.
The power of the Vltrasonic device described in step a is 200W ~ 500W, and ultrasonic time is 0.5 ~ 2.0h.
Concentration 0.1 ~ the 2.0mg/mL of graphene oxide in graphene oxide suspension described in step a.
Cyanamide concentration of aqueous solution described in step b is 20wt% ~ 50wt%.
Cyanamide described in step b and the mass ratio of graphene oxide are 1 ~ 5:80.
Solvent heat treatment temperature described in step b is 160 ~ 200 DEG C, and the time is 4 ~ 10 hours.
High-temperature process temperature described in step b is 600 ~ 100 DEG C, and the time is 1 ~ 6 hour.
Protective atmosphere described in step b is any one of nitrogen, argon gas, helium, neon, Krypton and xenon.
A kind of lithium battery, is characterized in that: have employed the lithium ion battery nitrogen-doped carbon coated graphite alkene material that right will go any one of 1-8 to prepare.
Tool of the present invention has the following advantages and beneficial effect:
(1) the nitrogen-doped carbon coated graphite alkene materials application that specific capacity is high, multiplying power is good that prepared by the present invention has no bibliographical information in lithium ion battery negative material, has good application development prospect.
(2) hydro-thermal one step of the present invention achieves the lithium ion battery negative material nitrogen-doped carbon coated graphite alkene material that nitrogen-doped carbon is prepared simultaneously.This kind of structural material can improve the specific area of nitrogen-doped carbon coated graphite alkene material, be conducive to the storage lithium specific capacity improving nitrogen-doped carbon coated graphite alkene material, contribute to the infiltration of electrolyte, prevent the reunion in Graphene reduction process, overlapping, thus improve the electronic conductivity of nitrogen-doped carbon coated graphite alkene material negative material, provide Research Thinking for seeking Novel cathode material for lithium ion battery.
(3) in the preparation process of lithium ion nitrogen-doped carbon coated graphite alkene material negative material: adopt hummer legal system for graphite oxide, then graphite oxide ultrasonic disperse is formed hydrophilic graphene oxide suspension in deionized water, surface of graphene oxide contains a large amount of carboxyls, hydroxyl, the oxy radicals such as carbonyl.Then add cyanamide, stir, put in closed reactor and carry out hydro-thermal reaction, under the high temperature and high pressure environment of reactor, can be there is aggregate packet and overlay on surface of graphene oxide in cyanamide, meanwhile, cyanamide also can be polymerized with the radical reaction of graphenic surface.Especially, graphene oxide is in whole hydrothermal reaction process, because the high temperature and high pressure environment of water heating kettle, occurs curling, fold under the effect of the oxy radical on surface and the reaction of cyanamide and intermolecular Van der Waals force etc., forms 3-D solid structure.Then presoma hydro-thermal obtained high temperature cabonization process under protective atmosphere obtains nitrogen-doped carbon coated graphite alkene material.
Accompanying drawing explanation
Fig. 1 is the projection Electronic Speculum figure (TEM) of graphene oxide.
Fig. 2 is the projection Electronic Speculum figure (TEM) of embodiment 1 nitrogen-doped carbon coated graphite alkene material and element mapping.
Fig. 3 is the charging and discharging curve of embodiment 1 nitrogen-doped carbon coated graphite alkene material under 0.01-3.0V, 200mA/g current density.
Fig. 4 is the cyclic curve of embodiment 1 nitrogen-doped carbon coated graphite alkene material under 0.01-3.0V, 200mA/g current density.
Fig. 5 is the circulation curve of embodiment 1 nitrogen-doped carbon coated graphite alkene material under 0.01-3.0V voltage.
Fig. 6 is the XRD collection of illustrative plates of embodiment 2 nitrogen-doped carbon coated graphite alkene material.
Fig. 7 is the cyclic curve of embodiment 2 nitrogen-doped carbon coated graphite alkene material under 0.01-3.0V, 200mA/g current density.
Fig. 8 is the circulation curve of embodiment 3 nitrogen-doped carbon coated graphite alkene material under 0.01-3.0V voltage.
Embodiment
In order to illustrate in greater detail the present invention, providing and followingly preparing example.But scope of the present invention is not limited thereto.
Embodiment 1, the preparation method of nitrogen-doped carbon coated graphite alkene material, comprises the following steps:
Adopt hummer legal system for graphite oxide, 80mg graphite oxide is formed graphene oxide suspension in ultrasonic 1 hour by the Ultrasound Instrument of 250W in 70mL deionized water, then the 10mL cyanamide aqueous solution (50wt%) is added, stir, put in 100mL reactor, 180 DEG C of hydro-thermal reactions 6 hours, hydro-thermal reaction product is spent deionized water, drying, 700 DEG C of high-temperature process 2 hours, obtain nitrogen-doped carbon coated graphite alkene material in a nitrogen atmosphere.
The electrochemical property test of lithium ion nitrogen-doped carbon coated graphite alkene material prepared by embodiment 1:
Lithium ion nitrogen-doped carbon coated graphite alkene material embodiment 1 prepared and conductive carbon black, binding agent Vingon (PVDF) to mix in mass ratio at 8: 1: 1, add appropriate 1-METHYLPYRROLIDONE (NMP) again to stir, be applied on Copper Foil, dry at 90 DEG C in vacuum drying oven, obtain nitrogen-doped carbon coated graphite alkene material electrodes sheet at sheet-punching machine top shear blade.The electrode obtained is done positive pole, metal lithium sheet is negative pole, electrolyte is for containing 1MLiPF6/ (EC+DMC) (volume ratio is 1: 1) mixed system, barrier film is microporous polypropylene membrane (Celgard2400), is assembled into 2025 type button cells in the glove box being full of argon gas (Ar).
Tester and method as follows:
Tem analysis instrument used is the microscopic appearance that the JSM-2010 type projection electron microscope (TEM) of NEC company observes specimen surface, and accelerating voltage is 200KV, and sample preparation drips on copper mesh after adopting absolute ethyl alcohol dispersion, air drying.
XRD analysis instrument used is the crystal phase structure material that Beijing Pu Xi all purpose instrument Co., Ltd XD-2 type X-ray diffractometer (XRD) characterizes prepared end product.Test condition is Cu target, K α radiation, and 36kV, 30mA walk wide by 0.02
o, sweep limits 10 ~ 80
o.Sample is that powder is placed in the pressing of sample stage groove, direct-detection.
Charge-discharge test instrument used is the BTS51800 battery test system of new Weir Electronics Co., Ltd. of Shenzhen, and model is CT-3008W, in 0.01-3.0V voltage range, carry out electro-chemical test.
As can be seen from Figure 1 the graphene oxide prepared is the lamellar structure of two dimension.As can be seen from Figure 2 hydro-thermal reaction rear oxidation Graphene is curling, and fold defines 3-D solid structure, and the nitrogen-doped carbon having glucose and cyanamide hydro-thermal to be formed on the surface of Graphene is coated, and element mapping shows that N doping is even.
Can find out that from Fig. 3,4 this material reaches 575mAh/g in first discharge specific capacity under 0.01-3.0V, 200mA/g current density, remain on 380mAh/g through 100 circulation specific discharge capacities.As can be seen from Figure 5 this material is at 0.01-3.0V, and the circulation performance under different current density is fine, and under 1680mA/g current density, specific discharge capacity reaches 248mAh/g.
Embodiment 2, the preparation method of lithium ion nitrogen-doped carbon coated graphite alkene material, comprises the following steps:
Adopt hummer legal system for graphite oxide, 80mg graphite oxide is formed graphene oxide suspension in ultrasonic 1 hour by the Ultrasound Instrument of 250W in 60mL deionized water, then the 20mL cyanamide aqueous solution (50wt%) is added, stir, put in 100mL reactor, 160 DEG C of hydro-thermal reactions 10 hours, hydro-thermal reaction product is spent deionized water, drying, 600 DEG C of high-temperature process 2 hours, obtain nitrogen-doped carbon coated graphite alkene material in a nitrogen atmosphere.
The electrochemical property test method of lithium ion nitrogen-doped carbon coated graphite alkene material prepared by embodiment 2 is identical with embodiment 1:
As can be seen from Figure 6 this material XRD collection of illustrative plates there is a steamed bun peak at about 23 °, this is the typical characteristic peak of glucose hydro-thermal carbon, do not occur that the characteristic peak of Graphene is because the content of Graphene is few in composite material, and graphene dispersion is good.As can be seen from Figure 7 this material first discharge specific capacity under 0.01-3.0V, 200mA/g current density reaches 475mAh/g, remains on 362.5mAh/g through 100 circulation specific discharge capacities.
Embodiment 3, the preparation method of lithium ion nitrogen-doped carbon coated graphite alkene material, comprises the following steps:
Adopt hummer legal system for graphite oxide, 80mg graphite oxide is formed graphene oxide suspension in ultrasonic 1.5 hours by the Ultrasound Instrument of 250W in 65mL deionized water, then the 15mL cyanamide aqueous solution (50wt%) is added, stir, put in 100mL reactor, 170 DEG C of hydro-thermal reactions 8 hours, hydro-thermal reaction product is spent deionized water, drying, 800 DEG C of high-temperature process 2 hours, obtain nitrogen-doped carbon coated graphite alkene material in a nitrogen atmosphere.
The electrochemical property test method of lithium ion nitrogen-doped carbon coated graphite alkene material prepared by embodiment 3 is identical with embodiment 1:
As can be seen from Figure 8 this material is at 0.01-3.0V, and the circulation performance under different current density is fine, and under 1680mA/g current density, specific discharge capacity reaches 180mAh/g.
Comparative example 1, the preparation method of lithium ion nitrogen-doped carbon coated graphite alkene material, comprises the following steps:
Adopt hummer legal system for graphite oxide, 80mg graphite oxide is formed graphene oxide suspension in ultrasonic 1.5 hours by the Ultrasound Instrument of 250W in 65mL deionized water, put in 100mL reactor, 170 DEG C of hydro-thermal reactions 8 hours, hydro-thermal reaction product is spent deionized water, drying, 800 DEG C of high-temperature process 2 hours, obtain grapheme material in a nitrogen atmosphere.
The electrochemical property test method of grapheme material prepared by comparative example 1 is identical with embodiment 1:
Circulation poor-performing under different current density, specific discharge capacity is less than 130mAh/g.
Can be drawn by data, lithium ion battery prepared by the lithium ion nitrogen-doped carbon coated graphite alkene material obtained by preparation method of the present invention, circulation excellent performance under the electric density of difference, has obvious advantage compared with comparative example.
The above; be only the present invention's preferably embodiment, but protection scope of the present invention is not limited thereto, any those of ordinary skill in the art are in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection range of claim.
Claims (9)
1. a preparation method for lithium ion battery nitrogen-doped carbon coated graphite alkene material, is characterized in that comprising the following steps:
A, preparation graphene oxide suspension: adopt hummer legal system for graphite oxide, by graphite oxide ultrasonic strip off formation graphene oxide suspension in deionized water;
B, prepare nitrogen-doped carbon coated graphite alkene material: in graphene oxide suspension, add a certain amount of cyanamide aqueous solution; stir; put into closed reactor and carry out hydro-thermal reaction; hydro-thermal reaction product is spent deionized water; dry; high-temperature process under protective atmosphere, obtains lithium ion battery nitrogen-doped carbon coated graphite alkene material.
2. the preparation method of lithium ion battery nitrogen-doped carbon coated graphite alkene material according to claim 1, is characterized in that: the power of the Vltrasonic device described in step a is 200W ~ 500W, and ultrasonic time is 0.5 ~ 2.0h.
3. the preparation method of lithium ion battery nitrogen-doped carbon coated graphite alkene material according to claim 1, is characterized in that: the concentration 0.1 ~ 2.0mg/mL of graphene oxide in the graphene oxide suspension described in step a.
4. the preparation method of lithium ion battery nitrogen-doped carbon coated graphite alkene material according to claim 1, is characterized in that: the cyanamide concentration of aqueous solution described in step b is 20wt% ~ 50wt%.
5. the preparation method of lithium ion battery nitrogen-doped carbon coated graphite alkene material according to claim 1, is characterized in that: the cyanamide described in step b and the mass ratio of graphene oxide are 1 ~ 5:80.
6. the preparation method of lithium ion battery nitrogen-doped carbon coated graphite alkene material according to claim 1, it is characterized in that: the solvent heat treatment temperature described in step b is 160 ~ 200 DEG C, the time is 4 ~ 10 hours.
7. the preparation method of lithium ion battery nitrogen-doped carbon coated graphite alkene material according to claim 1, it is characterized in that: the high-temperature process temperature described in step b is 600 ~ 100 DEG C, the time is 1 ~ 6 hour.
8. the preparation method of lithium ion battery nitrogen-doped carbon coated graphite alkene material according to claim 1, is characterized in that: the protective atmosphere described in step b is any one of nitrogen, argon gas, helium, neon, Krypton and xenon.
9. a lithium battery, is characterized in that: have employed lithium ion battery nitrogen-doped carbon coated graphite alkene material prepared by any one of claim 1-8.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108281654A (en) * | 2018-01-25 | 2018-07-13 | 东莞市迈科新能源有限公司 | A kind of preparation method of the high nitrogen doped anode material of lithium-ion battery of low temperature |
| CN108735999A (en) * | 2018-05-29 | 2018-11-02 | 上海应用技术大学 | A kind of preparation method and applications of the graphene-based N doping carbon-coating composite material of three-dimensional structure |
| CN109786771A (en) * | 2019-01-28 | 2019-05-21 | 西安科技大学 | A kind of preparation method of N doping three-dimensional grapheme base fuel battery cathod catalyst |
| CN113122878A (en) * | 2021-04-16 | 2021-07-16 | 陕西科技大学 | Nitrogen-doped carbon composite graphene coated metal cobalt catalyst, preparation method and application |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108281654A (en) * | 2018-01-25 | 2018-07-13 | 东莞市迈科新能源有限公司 | A kind of preparation method of the high nitrogen doped anode material of lithium-ion battery of low temperature |
| CN108735999A (en) * | 2018-05-29 | 2018-11-02 | 上海应用技术大学 | A kind of preparation method and applications of the graphene-based N doping carbon-coating composite material of three-dimensional structure |
| CN109786771A (en) * | 2019-01-28 | 2019-05-21 | 西安科技大学 | A kind of preparation method of N doping three-dimensional grapheme base fuel battery cathod catalyst |
| CN113122878A (en) * | 2021-04-16 | 2021-07-16 | 陕西科技大学 | Nitrogen-doped carbon composite graphene coated metal cobalt catalyst, preparation method and application |
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Application publication date: 20160511 |