CN109004186A - A kind of preparation method of multiple exotic atom doping three-dimensional grapheme - Google Patents
A kind of preparation method of multiple exotic atom doping three-dimensional grapheme Download PDFInfo
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- CN109004186A CN109004186A CN201810617923.XA CN201810617923A CN109004186A CN 109004186 A CN109004186 A CN 109004186A CN 201810617923 A CN201810617923 A CN 201810617923A CN 109004186 A CN109004186 A CN 109004186A
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- exotic atom
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- H—ELECTRICITY
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- 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
- H01M4/364—Composites as mixtures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- H—ELECTRICITY
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- 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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of multiple exotic atoms to adulterate three-dimensional grapheme, is obtained by following methods: will carry out hydro-thermal reaction containing the dispersion liquid of melamine and graphene oxide, obtains precast body；It by the exotic atom source with foreign atom and precast body mixed grinding, is calcined under atmosphere protection after grinding uniformly, obtains exotic atom doping three-dimensional grapheme.The carbon material has good high rate performance as lithium electricity and sodium electricity cathode, and large specific surface area and hierarchical porous structure are easily achieved load sulphur, can be used as the strong candidate material of lithium sulfur battery anode material.The preparation method is easy to operate, low in cost, it can be achieved that large scale preparation.This method can realize polyatom Uniform Doped, and doping and dopant states are controllable, be a kind of good negative electrode material in terms of lithium ion battery and sodium-ion battery.
Description
Technical field
The invention belongs to the technical fields of nano-carbon material, and in particular to a kind of multiple exotic atom doping three-dimensional grapheme
Preparation method.
Background technique
Carbon material due to electric conductivity height, abundance is low in cost, stable electrochemical property and be widely studied lithium electricity
Sodium electricity cathode field.A kind of two dimensional crystal of the graphene as single carbon atom thickness degree has been always by research since self-discovery
The favor of person, because theoretical and experimental results all show that graphene has highest electron mobility, thermal conductivity and machinery are strong
The physical and chemical performances such as degree.However graphene lacks intrinsic band gap and limits it the problem of easily stacking in an experiment again
Practical application in each field.Studies have shown that exotic atom doping can effectively open the band gap of graphene, so that physical chemistry
It is significantly improved with electric property.In addition, the regulation of graphene-structured three dimensional stress can be solved the problem of it is easily stacked.Common
Doped graphene method has CVD method, ball-milling method, plasma method, arc discharge method, wet chemistry method and heat treating process.It compares
Under, wet chemistry method occupies the advantages of experiment condition is simple and it can realize three dimensional gel carbon network and is widely used.Such as
A kind of high density nitrogen-doped graphene and preparation method thereof is disclosed in the patent that application publication number is CN105565306A.The party
Method reports graphene oxide and nitrogen source and is prepared for nitrogen-doped graphene by hydro-thermal method and applies on lithium electricity, compares graphene
Substantially increase the specific capacity of material.Although two-dimentional doped graphene can significantly improve the specific capacity of material as electrode material,
But it is kinetically still depositing by the space that has greatly improved.Much studies have shown that three-dimensional structure has the knot of perforation crosslinking
Structure, can effectively shorten the diffusion path of lithium ion or sodium ion, improve the dynamics of electrochemical reaction.
Summary of the invention
On the basis of existing issue, it is an object of the invention to propose that a kind of multiple exotic atom adulterates three-dimensional grapheme
Preparation method.The carbon material has a good high rate performance as lithium electricity and sodium electricity cathode, and large specific surface area and more
Grade pore structure is easily achieved load sulphur, can be used as the strong candidate material of lithium sulfur battery anode material.Preparation method operation letter
It is single, it is low in cost, it can be achieved that large scale preparation.This method can realize polyatom Uniform Doped, and doping and dopant states
It controllably, is a kind of good negative electrode material in terms of lithium ion battery and sodium-ion battery.
Specific technical solution is as follows: a kind of preparation method of multiple exotic atom doping three-dimensional grapheme includes the following steps:
(1) graphene oxide is dissolved in deionized water simultaneously ultrasonic disperse, and melamine is then added, stirs evenly, by the solution
It pours into 100ml polytetrafluoroethyllining lining, carries out hydro-thermal reaction, be dried after reaction, obtain precast body.The oxidation
The concentration of graphene aqueous solution is 0.5 ~ 7 mg/ml；The mass ratio of the graphene oxide and melamine is 3:1 ~ 10；It is described
The hydro-thermal reaction time is 4 ~ 18h, and hydrothermal temperature is 120 DEG C ~ 200 DEG C；The drying means is directly drying, freezes and do
One of dry, vacuum drying.
(2) exotic atom source and precast body are subjected to mixed grinding, are calcined under argon atmosphere protection after grinding uniformly.
The exotic atom source is one of trithiocyanuric acid, L-cysteine, selenium powder, bis- (diphenylphosphine) methane.The exotic atom
The mass ratio of source and precast body is 1 ~ 6:1；The calcination process uses heating rate for 2 ~ 15 DEG C/min, is warming up to 600 ~ 1200
DEG C and keep the temperature 1 ~ 6h.
The present invention using the preparation of above-mentioned process has following beneficial effect:
1. using template-free method, while realizing that three-dimensional structure is constructed, a variety of exotic atoms adulterate and manufacture hierarchical porous structure.It can
Pass through process control three-dimensional structure, doping and dopant states, the conspiracy relation of multi-stage porous three.Be beneficial to apply lithium from
Sub- battery and anode material of lithium-ion battery and as lithium-sulfur cell carry carbon material.
2. experimental implementation is easy, low in cost, it can be achieved that large scale preparation.
Detailed description of the invention
Fig. 1 is the stereoscan photograph of 4 honeycomb multi-stage porous nitrogen sulphur codope three-dimensional carbon material of embodiment.
Specific embodiment
Below with reference to embodiment, the present invention is further elaborated, but the present invention is not limited to following embodiment.
Embodiment 1:
(1) 40mg graphene oxide is dissolved in 80ml deionized water simultaneously ultrasonic disperse, 252mg melamine is then added, stirs
It mixes uniformly, pours this solution into 100ml polytetrafluoroethyllining lining, carry out 120 DEG C/12h of hydro-thermal reaction, carry out after reaction
Vacuum drying, obtains precast body.
(2) mass ratio by selenium powder and precast body with mass ratio for 2:1 carries out mixed grinding, in argon gas gas after grinding uniformly
600 DEG C are warming up to the heating rate of 2 DEG C/min under atmosphere protection and keep the temperature 3h.Obtain nitrogen selenium codope three-dimensional grapheme.
Embodiment 2:
(1) 100mg graphene oxide is dissolved in 50ml deionized water simultaneously ultrasonic disperse, 0.126g melamine is then added,
Stir evenly, pour this solution into 100ml polytetrafluoroethyllining lining, carry out 150 DEG C/18h of hydro-thermal reaction, after reaction into
Row vacuum drying, obtains precast body.
(2) mass ratio by selenium powder and precast body with mass ratio for 4:1 carries out mixed grinding, in argon gas gas after grinding uniformly
800 DEG C are warming up to the heating rate of 5 DEG C/min under atmosphere protection and keep the temperature 4h.Obtain nitrogen selenium codope three-dimensional grapheme.
Embodiment 3:
(1) 100mg graphene oxide is dissolved in 60ml deionized water simultaneously ultrasonic disperse, 0.126g melamine is then added,
Stir evenly, pour this solution into 100ml polytetrafluoroethyllining lining, carry out 180 DEG C/12h of hydro-thermal reaction, after reaction into
Row vacuum drying, obtains precast body.
(2) trithiocyanuric acid and precast body are subjected to mixed grinding with the mass ratio that mass ratio is 6:1, after grinding uniformly
1000 DEG C are warming up to the heating rate of 10 DEG C/min under argon atmosphere protection and keep the temperature 2h.Obtain nitrogen sulphur codope three-dimensional stone
Black alkene.
Referring to attached drawing 1, Fig. 1 is the SEM photograph that the present embodiment prepares sample.It is scanned with the S-4800 type of Japan Electronics Corporation
Electron microscope (SEM) carries out morphology observation, can significantly see that the three-dimensional structure constructed by nano-sheet substance is presented in sample.
Embodiment 4:
(1) 100mg graphene oxide is dissolved in 80ml deionized water simultaneously ultrasonic disperse, 0.063g melamine is then added,
Stir evenly, pour this solution into 100ml polytetrafluoroethyllining lining, carry out 200 DEG C/6h of hydro-thermal reaction, after reaction into
Row vacuum drying, obtains precast body.
(2) L-cysteine and precast body are subjected to mixed grinding with the mass ratio that mass ratio is 3:1, after grinding uniformly
900 DEG C are warming up to the heating rate of 15 DEG C/min under argon atmosphere protection and keep the temperature 3h.Obtain nitrogen sulphur codope three-dimensional stone
Black alkene.
Embodiment 5:
(1) 100mg graphene oxide is dissolved in 80ml deionized water simultaneously ultrasonic disperse, 0.084g melamine is then added,
Stir evenly, pour this solution into 100ml polytetrafluoroethyllining lining, carry out 200 DEG C/6h of hydro-thermal reaction, after reaction into
Row vacuum drying, obtains precast body.
(2) will be bis- (diphenylphosphine) methane and precast body mixed grinding carried out with the mass ratio that mass ratio is 2:1, grinding is equal
900 DEG C are warming up to the heating rate of 15 DEG C/min under argon atmosphere protection after even and keep the temperature 3h.Obtain nitrogen-phosphor codoping
Three-dimensional grapheme.
Embodiment 6:
(1) 30mg graphene oxide is dissolved in 60ml deionized water simultaneously ultrasonic disperse, 100mg melamine is then added, stirs
It mixes uniformly, pours this solution into 100ml polytetrafluoroethyllining lining, carry out 200 DEG C/4h of hydro-thermal reaction, carry out after reaction
Vacuum drying, obtains precast body.
(2) will be bis- (diphenylphosphine) methane and precast body mixed grinding carried out with the mass ratio that mass ratio is 6:1, grinding is equal
600 DEG C are warming up to the heating rate of 15 DEG C/min under argon atmosphere protection after even and keep the temperature 6h.Obtain nitrogen-phosphor codoping
Three-dimensional grapheme.
Embodiment 7:
(1) 210mg graphene oxide is dissolved in 30ml deionized water simultaneously ultrasonic disperse, 70mg melamine is then added, stirs
It mixes uniformly, pours this solution into 100ml polytetrafluoroethyllining lining, carry out 120 DEG C/18h of hydro-thermal reaction, carry out after reaction
Vacuum drying, obtains precast body.
(2) will be bis- (diphenylphosphine) methane and precast body mixed grinding carried out with the mass ratio that mass ratio is 1:1, grinding is equal
1200 DEG C are warming up to the heating rate of 15 DEG C/min under argon atmosphere protection after even and keep the temperature 1h.Obtain nitrogen-phosphor codoping
Three-dimensional grapheme.
Claims (8)
1. a kind of preparation method of multiple exotic atom doping three-dimensional grapheme, which comprises the steps of:
Hydro-thermal reaction will be carried out containing the dispersion liquid of melamine and graphene oxide, obtains precast body；It will be with foreign atom
Exotic atom source and precast body mixed grinding are calcined under atmosphere protection after grinding uniformly, are obtained exotic atom and are adulterated three-dimensional stone
Black alkene.
2. a kind of preparation method of multiple exotic atom doping three-dimensional grapheme according to claim 1, it is characterised in that: oxygen
The mass ratio of graphite alkene and melamine is 3:(1 ~ 10).
3. a kind of preparation method of multiple exotic atom doping three-dimensional grapheme according to claim 1, it is characterised in that: water
The thermal response time is 4 ~ 18h, and hydrothermal temperature is 120 DEG C ~ 200 DEG C.
4. a kind of preparation method of multiple exotic atom doping three-dimensional grapheme according to claim 1, it is characterised in that: institute
Stating exotic atom source is one of trithiocyanuric acid, L-cysteine, selenium powder, bis- (diphenylphosphine) methane or a variety of.
5. a kind of preparation method of multiple exotic atom doping three-dimensional grapheme according to claim 1, it is characterised in that: institute
The mass ratio for stating exotic atom source and precast body is (1 ~ 6): 1.
6. a kind of preparation method of multiple exotic atom doping three-dimensional grapheme according to claim 1, it is characterised in that: forge
It burns atmosphere to be protected using argon gas, calcination temperature is 600 ~ 1200 DEG C, and calcination time is 1 ~ 6h.
7. a kind of preparation method of multiple exotic atom doping three-dimensional grapheme according to claim 1, which is characterized in that tool
Body step includes:
1) graphene oxide is dissolved in deionized water simultaneously ultrasonic disperse, and melamine is then added, stirs evenly, which is fallen
Enter in 100ml polytetrafluoroethyllining lining, carries out hydro-thermal reaction, be dried after reaction, obtain precast body；The oxidation stone
The concentration of black aqueous solution is 0.5 ~ 7 mg/ml；The mass ratio of the graphene oxide and melamine is 3:1 ~ 10；The water
The thermal response time is 4 ~ 18h, and hydrothermal temperature is 120 DEG C ~ 200 DEG C；The drying means be directly drying, freeze-drying,
One of vacuum drying；
2) exotic atom source and precast body are subjected to mixed grinding, are calcined under argon atmosphere protection after grinding uniformly；It is described
Exotic atom source is one of trithiocyanuric acid, L-cysteine, selenium powder, bis- (diphenylphosphine) methane；The exotic atom source and
The mass ratio of precast body is 1 ~ 6:1；The calcination process uses heating rate for 2 ~ 15 DEG C/min, is warming up to 600 ~ 1200 DEG C simultaneously
Keep the temperature 1 ~ 6h.
8. the multiple exotic atom of any one of claim 1 ~ 7 the method preparation adulterates three-dimensional grapheme.
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| CN109516451A (en) * | 2018-12-27 | 2019-03-26 | 陕西科技大学 | A kind of preparation method of L-cysteine auxiliary synthesis three-dimensional grapheme |
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