CN109037678A - A kind of preparation method of nitrogen sulphur codope three-dimensional graphene foam electrode active material - Google Patents
A kind of preparation method of nitrogen sulphur codope three-dimensional graphene foam electrode active material Download PDFInfo
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- CN109037678A CN109037678A CN201810617854.2A CN201810617854A CN109037678A CN 109037678 A CN109037678 A CN 109037678A CN 201810617854 A CN201810617854 A CN 201810617854A CN 109037678 A CN109037678 A CN 109037678A
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- 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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- C01B32/00—Carbon; Compounds thereof
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- 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
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- H01M10/00—Secondary cells; Manufacture thereof
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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
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- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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Abstract
The invention discloses a kind of preparation methods of nitrogen sulphur codope three-dimensional graphene foam electrode material, include the following steps: to be immersed in nickel foam in the dispersion liquid including graphene oxide, melamine, trithiocyanuric acid and sufficient solvent, solvent thermal reaction；500 ~ 1200 DEG C of heat treatment solvent thermal reaction products under inert atmosphere；The nickel foam in heat-treated products is etched by strong acid, obtains nitrogen sulphur codope three-dimensional graphene foam.Based on the nitrogen sulphur codope three-dimensional graphene foam electrode material of above method preparation, there is three-dimensional doped graphene foam, and nitrogen, the element sulphur of doping；The nitrogen element content of doping in 3 ~ 7%, sulfur content in 1 ~ 3%, oxygen content 4 ~ 12%, doping is controllable.Experimental method is safe and non-toxic, low in cost, easy to operate.Prepared doping three-dimensional doped graphene foam electrode can have broad application prospects in lithium ion battery, the application of the fields such as supercapacitor and electro-catalysis.
Description
Technical field
The present invention relates to Graphene electrodes field of material technology, in particular to a kind of nitrogen sulphur codope three-dimensional graphene foam
The preparation method of electrode material.
Background technique
It is well known that graphene is a kind of two dimension crystalline substance of monoatomic layer thickness being made of carbon atom with perfect structure
Body.However graphene lacks intrinsic band gap and limits it in the reality in each field the problem of easily stacking in an experiment again
Using.Studies have shown that exotic atom doping can effectively open the band gap of graphene, so that physical chemistry and electric property obtain
It is apparent to improve.In addition, the regulation of graphene-structured three dimensional stress can be solved the problem of it is easily stacked.Common doped graphene method
There are CVD method, ball-milling method, plasma method, arc discharge method, wet chemistry method and heat treating process.In contrast, wet chemistry method accounts for
It is widely used according to experiment condition simple the advantages of simultaneously it can realize three dimensional gel carbon network.
In the energy such as lithium ion battery and sodium-ion battery direction, doped graphene has had excellent chemical property
It is widely studied a kind of highly dense to be disclosed in the patent of CN105565306A as a kind of electrode material, such as application publication number
Spend nitrogen-doped graphene and preparation method thereof.This method reports graphene oxide and nitrogen source and is prepared for N doping by hydro-thermal method
Graphene is simultaneously applied on lithium electricity, compared to the specific capacity that graphene improves material.Two-dimentional doped graphene is as electrode material
Although the specific capacity of material can be significantly improved, kinetically still depositing by the space that has greatly improved.Many research tables
Bright, three-dimensional structure has the structure of perforation crosslinking, can effectively shorten the diffusion path of lithium ion or sodium ion, improves electrochemistry
The dynamics of reaction.
Summary of the invention
It, should it is an object of the invention to propose a kind of preparation method of nitrogen sulphur codope three-dimensional graphene foam electrode material
Method is easy to operate, safe and non-toxic.Product large specific surface area has the advantages that while realizing doping and construction three-dimensional structure.It can
It applies in the energy such as lithium ion battery and sodium-ion battery direction, and can be used as carbon carrier sulfur loaded or selenium for lithium sulphur or lithium
Selenium cell anode.It can be applicable to lithium ion battery and sodium-ion battery field using electrode prepared by the method, and can be used as
Carbon carrier sulfur loaded or selenium are for lithium sulphur or lithium selenium cell anode.
Specific technical solution is as follows: a kind of preparation method of nitrogen sulphur codope three-dimensional graphene foam electrode material, including
Following steps:
(1) it graphene oxide and will be scattered in deionized water and alcohol mixed solvent, obtain graphene oxide dispersion, then
Melamine and trithiocyanuric acid are sequentially added, is stirred evenly.
(2) nickel foam is directly cut to the size of 30*60mm, immerses in the liquid of (1), is then charged into poly- the four of 100ml
Hydro-thermal reaction is carried out in vinyl fluoride reaction kettle.
(3) after the completion of hydro-thermal, product is freeze-dried, finally under protection of argon gas, is heat-treated in tube furnace.
(4) after the completion of being heat-treated, place the product in 5% dilute hydrochloric acid, nickel foam is etched away.After multiple centrifuge washing
Sample is dried, nitrogen sulphur codope three-dimensional graphene foam had both been obtained.
Specific graphene oxide, melamine trithiocyanuric acid and mass ratio are 1:0.2 ~ 2:0.2 ~ 2.5.Mixed solvent
Deionized water and the volume ratio of ethyl alcohol are 1 ~ 7:1.
The nickel foam is with a thickness of 0.5 ~ 2 mm.
In the hydro-thermal reaction, the hydro-thermal reaction time is 4 ~ 36 h, and hydrothermal temperature is 100 DEG C ~ 200 DEG C.
In heat treatment, heating rate is 2 ~ 20 DEG C/min, and heat treatment temperature is 500 ~ 1200 DEG C, and the time is the h of 1 h ~ 5.
The present invention prepared using above-mentioned process has following beneficial effect:
The present invention uses melamine and trithiocyanuric acid dopant, realizes that nitrogen, sulphur, oxygen are more in hydro-thermal reaction and heat treatment journey
Element doping.Simultaneously using nickel foam as matrix, gather melamine and trithiocyanuric acid in nickel foam
Symphysis is long, and graphene oxide, realizes the catalyzed graphitization of hard carbon material simultaneously during the high temperature treatment process, generates graphitization
The high three-dimensional doped graphene foam of degree.The invention has the advantages that using hydro-thermal method simultaneously realize doping, construction three-dimensional structure,
And catalyzed graphitization.Product nitrogen element content is 3 ~ 7%, and sulfur content is 1 ~ 3%, and for oxygen content 4 ~ 12%, doping can
Control；And experimental method is safe and non-toxic, low in cost, easy to operate.Prepared doping three-dimensional doped graphene foam electrode,
It can be in lithium ion battery, the application of the fields such as supercapacitor and electro-catalysis.Therefore method provided by the invention has wide
Application prospect.
Detailed description of the invention
Fig. 1 is the low power stereoscan photograph that embodiment 3 does not etch nickel foam；
Fig. 2 is that embodiment 3 etches away the stereoscan photograph after nickel foam；
Fig. 3 is the X ray diffracting spectrum of 3 nitrogen sulphur codope three-dimensional graphene foam 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) first 50mg graphene oxide is dispersed in the in the mixed solvent of 70ml deionized water and 10ml ethyl alcohol, is aoxidized
Graphene dispersing solution sequentially adds 0.03g melamine and 0.04g trithiocyanuric acid after ultrasound removes graphene oxide,
80 DEG C of stirrings are to being completely dissolved.
(2) nickel foam of 30*60*0.5mm is immersed in the liquid of (1), is then charged into the polytetrafluoroethyl-ne alkene reaction of 100ml
Hydro-thermal reaction is carried out in kettle.The hydro-thermal reaction time is 4h, and hydrothermal temperature is 100 DEG C.
(3) hydrothermal product freeze-drying is placed in tube furnace, with the heating speed of 2 DEG C/min under the atmosphere of argon gas protection
Rate is warming up to 500 DEG C of heat preservation 5h.
(4) by product leaching with 5% dilute hydrochloric acid, 80 DEG C of magnetic agitation 12h etch away nickel foam.It is then centrifuged for washing 6
It is secondary, it dries and sample is made.
Embodiment 2:
(1) first 100mg graphene oxide is dispersed in the in the mixed solvent of 25ml deionized water and 25ml ethyl alcohol, is aoxidized
Graphene dispersing solution, then sequentially adds 0.03g melamine and 0.04g trithiocyanuric acid, and 80 DEG C of stirrings are to being completely dissolved.
(2) nickel foam of 30*60*1mm is immersed in the liquid of (1), is then charged into the ptfe autoclave of 100ml
Middle carry out hydro-thermal reaction.The hydro-thermal reaction time is that for 24 hours, hydrothermal temperature is 150 DEG C.
(3) hydrothermal product freeze-drying is placed in tube furnace, with the heating speed of 5 DEG C/min under the atmosphere of argon gas protection
Rate is warming up to 600 DEG C of heat preservation 2h.
(4) by product leaching with 5% dilute hydrochloric acid, 80 DEG C of magnetic agitation 12h etch away nickel foam.It is then centrifuged for washing 6
It is secondary, it dries and sample is made.
Embodiment 3:
(1) first 100mg graphene oxide is dispersed in the in the mixed solvent of 50ml deionized water and 10ml ethyl alcohol, is aoxidized
Graphene dispersing solution, then sequentially adds 0.12g melamine and 0.17g trithiocyanuric acid, and 80 DEG C of stirrings are to being completely dissolved.
(2) nickel foam of 30*60*2mm is immersed in the liquid of (1), is then charged into the ptfe autoclave of 100ml
Middle carry out hydro-thermal reaction.The hydro-thermal reaction time is 36h, and hydrothermal temperature is 200 DEG C.
(3) hydrothermal product freeze-drying is placed in tube furnace, with the heating of 10 DEG C/min under the atmosphere of argon gas protection
Rate is warming up to 800 DEG C of heat preservation 1h.
(4) by product leaching with 5% dilute hydrochloric acid, 80 DEG C of magnetic agitation 12h etch away nickel foam.It is then centrifuged for washing 6
It is secondary, it dries and sample is made.
Referring to attached drawing 1 ~ 3, Fig. 1 is that nitrogen sulphur codope three-dimensional graphene foam prepared by the implementation case does not etch foam
The low power stereoscan photograph of nickel.Fig. 2 is the high power stereoscan photograph for etching away nickel foam, using the S- of Japan Electronics Corporation
4800 type scanning electron microscope (SEM) carry out morphology observation, it can be seen that significantly form three-dimensional structure by graphene nanometer sheet.
Fig. 3 is the X ray diffracting spectrum of nitrogen sulphur codope three-dimensional graphene foam, and the bright nickel foam of the chart is etched completely, only
Carbon material is left, it should be in the characteristic peak that the steamed bun peak of 2-Theta=23 ° is carbon material.
Embodiment 4:
(1) first 100mg graphene oxide is dispersed in the in the mixed solvent of 50ml deionized water and 20ml ethyl alcohol, is aoxidized
Graphene dispersing solution, then sequentially adds 0.18g melamine and 0.25g trithiocyanuric acid, and 80 DEG C of stirrings are to being completely dissolved.
(2) nickel foam of 30*60*0.5mm is immersed in the liquid of (1), is then charged into the polytetrafluoroethyl-ne alkene reaction of 100ml
Hydro-thermal reaction is carried out in kettle.The hydro-thermal reaction time is 12h, and hydrothermal temperature is 180 DEG C.
(3) hydrothermal product freeze-drying is placed in tube furnace, with the heating of 15 DEG C/min under the atmosphere of argon gas protection
Rate is warming up to 1000 DEG C of heat preservation 1h.
(4) by product leaching with 5% dilute hydrochloric acid, 80 DEG C of magnetic agitation 12h etch away nickel foam.It is then centrifuged for washing 6
It is secondary, it dries and sample is made.
Embodiment 5:
(1) first 100mg graphene oxide is dispersed in the in the mixed solvent of 40ml deionized water and 40ml ethyl alcohol, is aoxidized
Graphene dispersing solution, then sequentially adds 0.12g melamine and 0.08g trithiocyanuric acid, and 80 DEG C of stirrings are to being completely dissolved.
(2) nickel foam of 30*60*1mm is immersed in the liquid of (1), is then charged into the ptfe autoclave of 100ml
Middle carry out hydro-thermal reaction.The hydro-thermal reaction time is that for 24 hours, hydrothermal temperature is 120 DEG C.
(3) hydrothermal product freeze-drying is placed in tube furnace, with the heating of 20 DEG C/min under the atmosphere of argon gas protection
Rate is warming up to 900 DEG C of heat preservation 2h.
(4) by product leaching with 5% dilute hydrochloric acid, 80 DEG C of magnetic agitation 12h etch away nickel foam.It is then centrifuged for washing 6
It is secondary, it dries and sample is made.
Embodiment 6:
(1) first 100mg graphene oxide is dispersed in the in the mixed solvent of 70ml deionized water and 10ml ethyl alcohol, is aoxidized
Graphene dispersing solution, then sequentially adds 0.02g melamine and 0.02g trithiocyanuric acid, and 80 DEG C of stirrings are to being completely dissolved.
(2) nickel foam of 30*60*0.5mm is immersed in the liquid of (1), is then charged into the polytetrafluoroethyl-ne alkene reaction of 100ml
Hydro-thermal reaction is carried out in kettle.The hydro-thermal reaction time is 36h, and hydrothermal temperature is 100 DEG C.
(3) hydrothermal product freeze-drying is placed in tube furnace, with the heating of 20 DEG C/min under the atmosphere of argon gas protection
Rate is warming up to 500 DEG C of heat preservation 5h.
(4) by product leaching with 5% dilute hydrochloric acid, 80 DEG C of magnetic agitation 12h etch away nickel foam.It is then centrifuged for washing 6
It is secondary, it dries and sample is made.
Embodiment 7:
(1) first 100mg graphene oxide is dispersed in the in the mixed solvent of 40ml deionized water and 40ml ethyl alcohol, is aoxidized
Graphene dispersing solution, then sequentially adds 0.2g melamine and 0.25g trithiocyanuric acid, and 80 DEG C of stirrings are to being completely dissolved.
(2) nickel foam of 30*60*2mm is immersed in the liquid of (1), is then charged into the ptfe autoclave of 100ml
Middle carry out hydro-thermal reaction.The hydro-thermal reaction time is 4h, and hydrothermal temperature is 200 DEG C.
(3) hydrothermal product freeze-drying is placed in tube furnace, with the heating of 20 DEG C/min under the atmosphere of argon gas protection
Rate is warming up to 1200 DEG C of heat preservation 1h.
(4) by product leaching with 5% dilute hydrochloric acid, 80 DEG C of magnetic agitation 12h etch away nickel foam.It is then centrifuged for washing 6
It is secondary, it dries and sample is made.
Claims (7)
1. a kind of preparation method of nitrogen sulphur codope three-dimensional graphene foam electrode material, which comprises the steps of:
Nickel foam is immersed in the dispersion liquid including graphene oxide, melamine, trithiocyanuric acid and sufficient solvent, is carried out molten
Agent thermal response；500 ~ 1200 DEG C of heat treatment solvent thermal reaction products under inert atmosphere；Etching removes the foam in heat-treated products
Nickel obtains nitrogen sulphur codope three-dimensional graphene foam.
2. a kind of preparation method of nitrogen sulphur codope three-dimensional graphene foam electrode material according to claim 1, special
Sign is: in the dispersion liquid including graphene oxide, melamine, trithiocyanuric acid and sufficient solvent, graphite oxide
The mass ratio of alkene, melamine and trithiocyanuric acid be 1:(0.2 ~ 2): (0.2 ~ 2.5), the solvent be volume ratio be (1 ~
7): 1 water and the mixed solution of ethyl alcohol.
3. a kind of preparation method of nitrogen sulphur codope three-dimensional graphene foam electrode material according to claim 1, special
Sign is: the solvent thermal reaction time is 4 ~ 36 h, and solvent heat temperature is 100 DEG C ~ 200 DEG C.
4. a kind of preparation method of nitrogen sulphur codope three-dimensional graphene foam electrode material according to claim 1, special
Sign is: heat treatment temperature is 500 ~ 1200 DEG C, and heat treatment time is the h of 1 h ~ 5, and heat-treating atmosphere is argon gas.
5. a kind of preparation method of nitrogen sulphur codope three-dimensional graphene foam electrode material according to claim 1, special
Sign is that specific steps include:
1) disperse graphene oxide in deionized water and alcohol mixed solvent, obtain graphene oxide dispersion, then according to
Secondary addition melamine and trithiocyanuric acid, stir evenly；
2) nickel foam is directly cut to the size of 30*60mm, is immersed in the liquid of step 1), the polytetrafluoro of 100ml is then charged into
Hydro-thermal reaction is carried out in ethylene reaction kettle；
3) after the completion of hydro-thermal, product is freeze-dried, finally under protection of argon gas, is heat-treated in tube furnace；
4) after the completion of being heat-treated, place the product in 5% dilute hydrochloric acid, nickel foam is etched away；Sample is dried after multiple centrifuge washing
Product had both obtained nitrogen sulphur codope three-dimensional graphene foam；
The nickel foam is with a thickness of 0.5 ~ 2 mm；
The heat treatment heating rate is 2 ~ 20 DEG C/min.
6. the nitrogen sulphur codope three-dimensional graphene foam electrode material that any one of claim 1 ~ 5 the method obtains.
7. a kind of nitrogen sulphur codope three-dimensional graphene foam electrode material according to claim 6, it is characterised in that: including
Three-dimensional doped graphene foam and the nitrogen of doping, element sulphur；The nitrogen element content of the doping is in 3 ~ 7%, sulfur content 1
~ 3%, for oxygen content 4 ~ 12%, doping is controllable.
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| CN109980210A (en) * | 2019-04-19 | 2019-07-05 | 陕西科技大学 | A kind of niobium pentaoxide three-dimensional doped graphene composite material and preparation method and application |
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| CN115050943A (en) * | 2022-07-12 | 2022-09-13 | 北京北化工程技术有限公司 | Selenium-doped thiotrithiocyanuric acid material with high compaction density, preparation method thereof and battery positive plate |
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