CN109019565A - A kind of preparation method of three-dimensional porous nitrogen sulfur doping carbon nanosheet - Google Patents
A kind of preparation method of three-dimensional porous nitrogen sulfur doping carbon nanosheet Download PDFInfo
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- CN109019565A CN109019565A CN201810617891.3A CN201810617891A CN109019565A CN 109019565 A CN109019565 A CN 109019565A CN 201810617891 A CN201810617891 A CN 201810617891A CN 109019565 A CN109019565 A CN 109019565A
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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- 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
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Abstract
A kind of three-dimensional porous nitrogen sulfur doping carbon nanosheet, obtains by the following method: the homogeneous solution containing trithiocyanuric acid is slowly added in the graphene oxide water solution dissolved with melamine, be sufficiently stirred at 50 ~ 120 DEG C；Place the product in two sections of heating heat treatments are carried out under vacuum environment in 300 ~ 500 DEG C and 700 ~ 900 DEG C, be passed through inert atmosphere terminates up to cooling down, and obtains three-dimensional porous nitrogen sulfur doping carbon nanosheet.The present invention is built into three-dimensional carbon material in the presence of graphene by molecule aggregation formation carbon skeleton using melamine and trithiocyanuric acid are super jointly；Melamine, trithiocyanuric acid are used as the nitrogen source and sulphur source of nitrogen, sulfur doping simultaneously, carry out nitrogen, sulfur doping to graphene carbon material.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.The preparation method is easy to operate, low in cost, it can be achieved that large scale preparation.
Description
Technical field
The invention belongs to the technical fields of nano-carbon material, and in particular to a kind of three-dimensional porous nitrogen sulfur doping carbon nanosheet
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 a kind of three-dimensional porous nitrogen sulfur doping carbon nanosheet
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.The carbon material not only has the nitrogen sulphur atom of Uniform Doped, and specific surface area
It greatly, is a kind of good active material in terms of alkali metal-ion battery.
Specific technical solution is as follows: a kind of preparation method of three-dimensional porous nitrogen sulfur doping carbon nanosheet includes the following steps:
(1) graphene oxide deionized water solution ultrasonic disperse, is then added melamine, stirs evenly, and is denoted as A liquid.It is described
The concentration of graphene oxide water solution is 0.2 ~ 4 mg/ml.
(2) trithiocyanuric acid is dissolved in organic solvent, stirred evenly, be denoted as B liquid.The organic solvent is N-methyl pyrroles
One of alkanone, dimethylformamide, ethylenediamine, ethyl alcohol or dimethyl sulfoxide.The concentration of the trithiocyanuric acid solution is 7
~ 30 mg/ml, the mass ratio of the graphene oxide, melamine and trithiocyanuric acid are to go described in 1:0.3 ~ 4:0.4 ~ 7.
The volume ratio of ionized water and organic solvent is 1 ~ 5:1
(3) under conditions of magnetic agitation, B liquid is slowly dropped into A liquid, acquired solution is then subjected to heating water bath and is held
Continuous stirring.The time of heating water bath is 1h ~ for 24 hours, and temperature is 50 DEG C ~ 120 DEG C.
(4) it then by after sample drying, calcines under vacuum conditions.The drying means is vacuum drying, freeze-drying
Or baking oven drying.The calcination process uses heating rate for 5 ~ 25 DEG C/min, is warming up to 300 ~ 500 DEG C of 1 ~ 3h of heat preservation, so
700 ~ 900 DEG C of 0.5 ~ 2h of heat preservation are being warming up to the heating rate of 5 ~ 25 DEG C/min afterwards, last temperature-fall period is passed through argon gas.
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, nitrogen sulphur atom adulterates and manufacture hierarchical porous structure.It can lead to
Cross the conspiracy relation of process control three-dimensional structure, doping and dopant states, multi-stage porous three.It is beneficial to apply in lithium ion
Battery and anode material of lithium-ion battery and as lithium-sulfur cell carry carbon material.
2. use melamine and trithiocyanuric acid for nitrogen source and sulphur source, while the two supermolecule aggregates into carbon skeleton,
Under the participation of graphene, it is built into three-dimensional carbon material jointly.
3. 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 the three-dimensional nitrogen sulphur codope carbon material of embodiment 1.
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) 30mg graphene oxide is dissolved in 30ml deionized water, ultrasonic disperse, 0.063g melamine is then added, stirs
It mixes uniformly, is denoted as A liquid.
(2) 0.177g trithiocyanuric acid is dissolved in 30ml ethyl alcohol, is stirred evenly, be denoted as B liquid.
(3) under conditions of magnetic agitation, B liquid is slowly dropped into A liquid, then carries out acquired solution at 80 DEG C
Under the conditions of heating water bath 10h and continue to stir.
(4) sample is freeze-dried, is then warming up to 350 DEG C under vacuum conditions with the heating rate of 10 DEG C/min and protected
Warm 2h, is then warming up to 700 DEG C of heat preservation 2h again with same heating rate, and heat preservation end is passed through argon gas protection and cooled down
Journey.
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 porous three-dimensional manometer chip architecture.
Embodiment 2:
(1) 60mg graphene oxide is dissolved in 30ml deionized water, ultrasonic disperse, 0.063g melamine is then added, stirs
It mixes uniformly, is denoted as A liquid.
(2) 0.354g trithiocyanuric acid is dissolved in 15ml N-methyl pyrrolidones, is stirred evenly, be denoted as B liquid.
(3) under conditions of magnetic agitation, B liquid is slowly dropped into A liquid, then carries out acquired solution at 100 DEG C
Under the conditions of heating water bath 2h and continue to stir.
(4) sample is freeze-dried, is then warming up to 500 DEG C under vacuum conditions with the heating rate of 20 DEG C/min and protected
Warm 2h, is then warming up to 800 DEG C of heat preservation 1h again with same heating rate, and heat preservation end is passed through argon gas protection and cooled down
Journey.
Embodiment 3:
(1) 100mg graphene oxide is dissolved in 25ml deionized water, ultrasonic disperse, 0.126g melamine is then added, stirs
It mixes uniformly, is denoted as A liquid.
(2) 0.177g trithiocyanuric acid is dissolved in 20ml N-methyl pyrrolidones, is stirred evenly, be denoted as B liquid.
(3) under conditions of magnetic agitation, B liquid is slowly dropped into A liquid, then carries out acquired solution at 120 DEG C
Under the conditions of heating water bath 1h and continue to stir.
(4) sample is freeze-dried, is then warming up to 400 DEG C under vacuum conditions with the heating rate of 20 DEG C/min and protected
Warm 3h, is then warming up to 900 DEG C of heat preservation 0.5h again with same heating rate, and heat preservation end is passed through argon gas protection and cooled down
Journey.
Embodiment 4:
(1) 100mg graphene oxide is dissolved in 20ml deionized water, ultrasonic disperse, 0.084g melamine is then added, stirs
It mixes uniformly, is denoted as A liquid.
(2) 0.443g trithiocyanuric acid is dissolved in 10ml dimethylformamide, is stirred evenly, be denoted as B liquid.
(3) under conditions of magnetic agitation, B liquid is slowly dropped into A liquid, then carries out acquired solution at 60 DEG C
Under the conditions of heating water bath 2h and continue to stir.
(4) sample is freeze-dried, is then warming up to 500 DEG C under vacuum conditions with the heating rate of 5 DEG C/min and protected
Warm 2h, is then warming up to 800 DEG C of heat preservation 1h again with same heating rate, and heat preservation end is passed through argon gas protection and cooled down
Journey.
Embodiment 5:
(1) 80mg graphene oxide is dissolved in 40ml deionized water, ultrasonic disperse, 0.126g melamine is then added, stirs
It mixes uniformly, is denoted as A liquid.
(2) 0.177g trithiocyanuric acid is dissolved in 10ml N-methyl pyrrolidones, is stirred evenly, be denoted as B liquid.
(3) under conditions of magnetic agitation, B liquid is slowly dropped into A liquid, then carries out acquired solution at 80 DEG C
Under the conditions of heating water bath 1h and continue to stir.
(4) sample is freeze-dried, is then warming up to 400 DEG C under vacuum conditions with the heating rate of 20 DEG C/min and protected
Warm 3h, is then warming up to 700 DEG C of heat preservation 2h again with same heating rate, and heat preservation end is passed through argon gas protection and cooled down
Journey.
Embodiment 6:
(1) 8 mg graphene oxides are dissolved in 40 ml deionized waters, ultrasonic disperse, 32 mg melamines is then added, stir
It mixes uniformly, is denoted as A liquid.
(2) 56 mg trithiocyanuric acids are dissolved in 8 ml N-methyl pyrrolidones, stir evenly, is denoted as B liquid.
(3) under conditions of magnetic agitation, B liquid is slowly dropped into A liquid, then carries out acquired solution at 50 DEG C
Under the conditions of heating water bath for 24 hours and continue to stir.
(4) sample is freeze-dried, is then warming up to 300 DEG C under vacuum conditions with the heating rate of 20 DEG C/min and protected
Warm 3h, is then warming up to 700 DEG C of heat preservation 2h again with same heating rate, and heat preservation end is passed through argon gas protection and cooled down
Journey.
Embodiment 7:
(1) 160 mg graphene oxides are dissolved in 40 ml deionized waters, ultrasonic disperse, 48 mg melamines are then added,
It stirs evenly, is denoted as A liquid.
(2) 64 mg trithiocyanuric acids are dissolved in 8ml N-methyl pyrrolidones, are stirred evenly, be denoted as B liquid.
(3) under conditions of magnetic agitation, B liquid is slowly dropped into A liquid, then carries out acquired solution at 120 DEG C
Under the conditions of heating water bath 1h and continue to stir.
(4) sample is freeze-dried, is then warming up to 500 DEG C under vacuum conditions with the heating rate of 20 DEG C/min and protected
Warm 1h, is then warming up to 900 DEG C of heat preservation 0.5h again with same heating rate, and heat preservation end is passed through argon gas protection and cooled down
Journey.
Claims (9)
1. a kind of preparation method of three-dimensional porous nitrogen sulfur doping carbon nanosheet, which comprises the steps of:
Homogeneous solution containing trithiocyanuric acid is slowly added in the graphene oxide water solution dissolved with melamine, 50 ~ 120
It is sufficiently stirred at DEG C；Desciccate, place the product in, in 300 ~ 500 DEG C of 1 ~ 3h of heat preservation, then be warming up to 700 ~ 900 under vacuum environment
DEG C heat preservation 0.5 ~ 2h, be passed through inert atmosphere until cooling terminate, obtain three-dimensional porous nitrogen sulfur doping carbon nanosheet.
2. a kind of preparation method of three-dimensional porous nitrogen sulfur doping carbon nanosheet according to claim 1, it is characterised in that: oxygen
The mass ratio of graphite alkene, melamine and trithiocyanuric acid is 1:(0.3 ~ 4): (0.4 ~ 7).
3. a kind of preparation method of three-dimensional porous nitrogen sulfur doping carbon nanosheet according to claim 1, it is characterised in that: will
Mixed liquor including graphene oxide, melamine and trimerization hydrosulphuric acid 50 DEG C ~ 120 DEG C stir 1 ~ for 24 hours.
4. a kind of preparation method of three-dimensional porous nitrogen sulfur doping carbon nanosheet according to claim 1, it is characterised in that: contain
The solvent for having the homogeneous solution of trithiocyanuric acid is N-methyl pyrrolidones, dimethylformamide, ethylenediamine, ethyl alcohol or dimethyl
One of sulfoxide is a variety of.
5. a kind of preparation method of three-dimensional porous nitrogen sulfur doping carbon nanosheet according to claim 1, it is characterised in that: institute
The concentration for stating graphene oxide in the graphene oxide water solution dissolved with melamine is 0.2 ~ 4 mg/ml.
6. a kind of preparation method of three-dimensional porous nitrogen sulfur doping carbon nanosheet according to claim 1, it is characterised in that: institute
The concentration for stating trithiocyanuric acid solution is 7 ~ 30 mg/ml.
7. a kind of preparation method of three-dimensional porous nitrogen sulfur doping carbon nanosheet according to claim 1, which is characterized in that tool
Body step includes:
1) graphene oxide deionized water solution ultrasonic disperse, is then added melamine, stirs evenly, and is denoted as A liquid；The oxygen
The concentration of graphite aqueous solution is 0.2 ~ 4 mg/ml；
2) trithiocyanuric acid is dissolved in organic solvent, stirred evenly, be denoted as B liquid；The organic solvent be N-methyl pyrrolidones,
One of dimethylformamide, ethylenediamine, ethyl alcohol or dimethyl sulfoxide；The concentration of the trithiocyanuric acid solution is 7 ~ 30
mg/ml；The mass ratio of the graphene oxide, melamine and trithiocyanuric acid is 1:(0.3 ~ 4): (0.4 ~ 7)；It is described go from
The volume ratio of sub- water and organic solvent is (1 ~ 5): 1；
3) under conditions of magnetic agitation, B liquid is slowly dropped into A liquid, acquired solution is then subjected to heating water bath and is continued
Stirring；The time of heating water bath is 1h ~ for 24 hours, and temperature is 50 DEG C ~ 120 DEG C；
4) it then by after sample drying, calcines under vacuum conditions；The drying means is vacuum drying, freeze-drying or baking
Case drying；The calcination process uses heating rate for 5 ~ 25 DEG C/min, 300 ~ 500 DEG C of 1 ~ 3h of heat preservation is warming up to, then with 5
The heating rate of ~ 25 DEG C/min is warming up to 700 ~ 900 DEG C of 0.5 ~ 2h of heat preservation, and last temperature-fall period is passed through argon gas.
8. the three-dimensional porous nitrogen sulfur doping carbon nanosheet of any one of claim 1 ~ 7 the method preparation.
9. a kind of three-dimensional porous nitrogen sulfur doping carbon nanosheet according to claim 8, it is characterised in that: melamine and three
Polysulfide cyanic acid is super to be built into three-dimensional carbon material in the presence of graphene by molecule aggregation formation carbon skeleton jointly；While three
Poly cyanamid, trithiocyanuric acid are used as the nitrogen source and sulphur source of nitrogen, sulfur doping, carry out nitrogen, sulfur doping to graphene carbon material.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN109970043A (en) * | 2019-04-08 | 2019-07-05 | 中国石油大学(华东) | Nitrogen-phosphor codoping carbon nanosheet and preparation method thereof, alkali metal-ion battery electrode, alkali metal-ion battery and electric device |
| CN110048106A (en) * | 2019-04-19 | 2019-07-23 | 陕西科技大学 | A kind of cobalt sulfide and multistage carbon nano-structured composite material and preparation method and application |
| CN110775959A (en) * | 2019-10-31 | 2020-02-11 | 西北工业大学 | Preparation method for preparing nitrogen-sulfur co-doped porous graphene by supramolecular template method |
| CN115215320A (en) * | 2022-06-22 | 2022-10-21 | 广东工业大学 | Supramolecular induced nitrogen-doped lignin-derived carbon material and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109970043A (en) * | 2019-04-08 | 2019-07-05 | 中国石油大学(华东) | Nitrogen-phosphor codoping carbon nanosheet and preparation method thereof, alkali metal-ion battery electrode, alkali metal-ion battery and electric device |
| CN109970043B (en) * | 2019-04-08 | 2020-11-27 | 中国石油大学(华东) | Nitrogen-phosphorus co-doped carbon nanosheet and preparation method thereof, alkali metal ion battery electrode, alkali metal ion battery and electric device |
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| CN110775959A (en) * | 2019-10-31 | 2020-02-11 | 西北工业大学 | Preparation method for preparing nitrogen-sulfur co-doped porous graphene by supramolecular template method |
| CN115215320A (en) * | 2022-06-22 | 2022-10-21 | 广东工业大学 | Supramolecular induced nitrogen-doped lignin-derived carbon material and preparation method and application thereof |
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