CN109911889A - A kind of nitrogen sulphur codope porous graphene and its preparation method and application - Google Patents
A kind of nitrogen sulphur codope porous graphene and its preparation method and application Download PDFInfo
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- CN109911889A CN109911889A CN201910318113.9A CN201910318113A CN109911889A CN 109911889 A CN109911889 A CN 109911889A CN 201910318113 A CN201910318113 A CN 201910318113A CN 109911889 A CN109911889 A CN 109911889A
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Abstract
The present invention discloses a kind of nitrogen sulphur codope porous graphene and its preparation method and application, and preparation method is simply controllable, safe and non-toxic, exotic atom doping and mesoporous controllable quantity in preparation process, and exotic atom and pore size distribution provide storage lithium and store up the work site of sodium；The nitrogen sulphur codope porous graphene of preparation is used to store up lithium and storage sodium.In addition it adulterates site and pore structure is also the active site for adsorbing sulphur, can be used as the carrier for carrying sulphur in lithium-sulfur cell.Prepared nitrogen sulphur codope porous graphene, can be applied to lithium ion battery and sodium-ion battery negative electrode active material or lithium-sulfur cell carries the fields such as sulfur-donor.
Description
Technical field
The invention belongs to carbon nanomaterial field, it is related to the carbon nanometer that a kind of doped graphene and porous graphene combine
A kind of material, and in particular to nitrogen sulphur codope porous graphene and its preparation method and application.
Background technique
Graphene is a kind of two-dimensional material for having perfect electric conductivity, and in past ten years, graphene is changing always
The landscape of numerous science and technology fields, especially Condensed Matter Physics, energy storage and conversion and biomedical research etc. lead
Domain.It is at present still the hot topic of academia about the research for continuing exploration graphene and Graphene derivative potential ability.So
And lacks intrinsic band gap and catalytic capability and seem to significantly limit the practical application of graphene, but can be changed due to its structure
Shape and height adjustability, the legend of this 2D material are by sustainable development.
In addition, exotic atom doping can effectively open the band gap of graphene, so that physical chemistry and electric property obtain
It is apparent to improve, improve its application value as energy storage material.Studies have shown that doping is limited, on doped graphene
Pore-creating is a kind of new strategy for breaking doped graphene energy storage bottleneck.In existing research, using a kind of mild method
Realize that the research of doping and pore-creating is also fewer and fewer simultaneously on graphene.
Summary of the invention
To overcome above-mentioned the deficiencies in the prior art, it is an object of the present invention to provide a kind of nitrogen sulphur codope porous graphene and its
Preparation method and application, this method is safe and non-toxic, low in cost, easy to operate, and doping and pore size distribution are controllable.
To achieve the above object, the technical solution adopted by the present invention is that:
A kind of preparation method of nitrogen sulphur codope porous graphene, comprising the following steps:
(1) by graphene oxide, melamine, trithiocyanuric acid and transition metal nitrate be successively scattered in ethyl alcohol and
In the mixed solution of deionized water, it is stirred to react sufficiently；The graphene oxide, melamine, trithiocyanuric acid, transition metal
The mass ratio of nitrate is 1:(1.2~10): (1~15): (10~30)；The volume ratio of the middle ethyl alcohol and deionized water is 1:
(1~8)；
Then stirring product is transferred in water heating kettle and carries out hydro-thermal reaction；The time of the hydro-thermal reaction is 8-48h, water
Hot temperature is 80~200 DEG C；
(2) sample that hydro-thermal reaction terminates with deionized water filtering and washing for several times, then dry, dry sample be placed in
Calcination processing is carried out in the tube furnace of inert gas shielding；
In the calcination process, heating rate is 10~30 DEG C/min, and holding temperature is 400~1000 DEG C, soaking time
For 0~4h；
(3) transition metal material in heat-treated products is etched away with dilute hydrochloric acid, then filtering and washing product and drying, i.e.,
Obtain nitrogen sulphur codope porous graphene.
Further, the time that the step 1) is stirred to react is 0.1~2h, and whipping temp is 50~140 DEG C.
Further, transition metal nitrate is Nickelous nitrate hexahydrate, cabaltous nitrate hexahydrate and nine hydrations in the step 1)
One of ferric nitrate is a variety of.
Further, the packing ratio of hydro-thermal reaction is 40%~85% in the step 1).
Further, the heat treatment in the step 2), in the calcination process, the flow velocity of protective gas is 0-500sccm.
Further, it using the dilute hydrochloric acid of 0.5~5M when dilute hydrochloric acid etches in the step 3), etches 1-5 days.
Further, nitrogen atom doping amount is 2at%~10at%, sulphur atom doping in nitrogen sulphur codope porous graphene
For 0.2at%~3at%, mesoporous pore volume is 0.025-0.09cm3/g。
A kind of nitrogen sulphur codope porous graphene as cathode of lithium battery active material, sode cell negative electrode active material or
The application of lithium-sulfur cell load sulfur-donor.
Advantageous effect of the invention is embodied in:
The preparation method of nitrogen sulphur codope porous graphene of the invention, process is simply controllable, safe and non-toxic, preparation process
Middle exotic atom doping and mesoporous controllable quantity, exotic atom and pore size distribution provide storage lithium and store up the work site of sodium；Preparation
Nitrogen sulphur codope porous graphene is used to store up lithium and storage sodium.In addition it adulterates site and pore structure is also the active site for adsorbing sulphur,
It can be used as the carrier that sulphur is carried in lithium-sulfur cell.Prepared nitrogen sulphur codope porous graphene, can be applied to lithium ion battery and
Sodium-ion battery negative electrode active material or lithium-sulfur cell carry the fields such as sulfur-donor.
Detailed description of the invention
Fig. 1 is scanning electron microscopy (SEM) photo of nitrogen sulphur codope three-dimensional grapheme prepared by embodiment 4
Specific embodiment
The present invention is further elaborated With reference to embodiment, but the present invention is not limited to following implementation
Example.
Embodiment 1
(1) it disperses 0.1g graphene oxide in the mixed solution of 20ml deionized water and 10ml ethyl alcohol, then successively
0.12g melamine, six water nickel nitrate of 0.32g trithiocyanuric acid and 0.6g is added, continues to stir under conditions of 70 DEG C
30min.Then the solution is transferred in polytetrafluoroethyllining lining and carries out hydro-thermal reaction, 120 DEG C/8h of hydro-thermal reaction.By hydro-thermal
The sample that reaction terminates carries out multiple filtering and washing, freeze-drying, then with 10 DEG C/min's in the tube furnace of argon gas protection
Heating rate is warming up to 600 DEG C of heat preservation 0h, and the flow velocity of argon gas is 0sccm in heat treatment process.
(2) it etches transition metal material: heat-treated products is dissolved in stirring etching 5 in the dilute hydrochloric acid of the 0.5M of 20ml
It, then filtering and washing product and dry to get arriving nitrogen sulphur codope porous graphene.
Embodiment 2
(1) it disperses 0.1g graphene oxide in the mixed solution of 40ml deionized water and 40ml ethyl alcohol, then successively
0.24g melamine, six water nickel nitrate of 0.32g trithiocyanuric acid and 0.4g cobalt nitrate hexahydrate and 0.4g is added, in 50 DEG C of item
Continue to stir 120min under part.Then the solution is transferred in polytetrafluoroethyllining lining and carries out hydro-thermal reaction, hydro-thermal reaction 100
℃/24h.The sample that hydro-thermal reaction is terminated carries out multiple filtering and washing, freeze-drying, then in the tube furnace of argon gas protection
800 DEG C of heat preservation 1h are warming up to the heating rate of 15 DEG C/min, the flow velocity of argon gas is 100sccm in heat treatment process.
(2) it etches transition metal material: heat-treated products is dissolved in stirring etching 2 days in the dilute hydrochloric acid of the 1M of 20ml,
Then filtering and washing product and dry to get arriving nitrogen sulphur codope porous graphene.
Embodiment 3
(1) it disperses 0.05g graphene oxide in the mixed solution of 25ml deionized water and 25ml ethyl alcohol, then successively
0.35g melamine, 0.56g trithiocyanuric acid and 0.5g Fe(NO3)39H2O is added, continues to stir under conditions of 90 DEG C
100min.Then the solution is transferred in polytetrafluoroethyllining lining and carries out hydro-thermal reaction, 200 DEG C/8h of hydro-thermal reaction.By hydro-thermal
The sample that reaction terminates carries out multiple filtering and washing, freeze-drying, then with 20 DEG C/min's in the tube furnace of argon gas protection
Heating rate is warming up to 1000 DEG C of heat preservation 3h, and the flow velocity of argon gas is 300sccm in heat treatment process.
(2) it etches transition metal material: heat-treated products is dissolved in stirring etching 3 days in the dilute hydrochloric acid of the 5M of 20ml,
Then filtering and washing product and dry to get arriving nitrogen sulphur codope porous graphene.
Embodiment 4
(1) it disperses 0.12g graphene oxide in the mixed solution of 30ml deionized water and 10ml ethyl alcohol, then successively
0.96g melamine, six water nickel nitrate of 1.2g trithiocyanuric acid and 0.4g cobalt nitrate hexahydrate and 0.4g is added, in 60 DEG C of condition
Under continue stir 90min.Then the solution is transferred in polytetrafluoroethyllining lining and carries out hydro-thermal reaction, 180 DEG C of hydro-thermal reaction/
24h.The sample that hydro-thermal reaction is terminated carries out multiple filtering and washing, freeze-drying, then in the tube furnace of argon gas protection with
The heating rate of 20 DEG C/min is warming up to 900 DEG C of heat preservation 3h, and the flow velocity of argon gas is 150sccm in heat treatment process.
(2) it etches transition metal material: heat-treated products is dissolved in stirring etching 2 days in the dilute hydrochloric acid of the 3M of 20ml,
Then filtering and washing product and dry to get arriving nitrogen sulphur codope porous graphene.
Referring to Fig.1, Fig. 1 is the SEM photograph that the present embodiment prepares sample.Electricity is scanned with the S-4800 type of Japan Electronics Corporation
Sub- microscope (SEM) carries out morphology observation, and the pore structure of different-diameter is uniformly dispersed on the apparent three-dimensional grapheme of energy.
Embodiment 5
(1) it disperses 0.05g graphene oxide in the mixed solution of 30ml deionized water and 30ml ethyl alcohol, then successively
0.12g melamine, 0.53g trithiocyanuric acid and 0.8g Fe(NO3)39H2O and 0.8g cobalt nitrate hexahydrate is added, in 50 DEG C
Under the conditions of continue stir 120min.Then the solution is transferred in polytetrafluoroethyllining lining and carries out hydro-thermal reaction, hydro-thermal reaction
150℃/48h.The sample that hydro-thermal reaction is terminated carries out multiple filtering and washing, freeze-drying, then in the tubular type of argon gas protection
1000 DEG C of heat preservation 4h are warming up to the heating rate of 30 DEG C/min in furnace, the flow velocity of argon gas is in heat treatment process
500sccm。
(2) it etches transition metal material: heat-treated products is dissolved in stirring etching 4 days in the dilute hydrochloric acid of the 5M of 20ml,
Then filtering and washing product and dry to get arriving nitrogen sulphur codope porous graphene.
Embodiment 6
(1) it disperses 0.05g graphene oxide in the mixed solution of 50ml deionized water and 25ml ethyl alcohol, then successively
0.24g melamine, 0.17g trithiocyanuric acid and 1g cobalt nitrate hexahydrate is added, continues to stir 20min under conditions of 120 DEG C.
Then the solution is transferred in polytetrafluoroethyllining lining and carries out hydro-thermal reaction, the packing ratio of hydro-thermal reaction is 70%, and hydro-thermal is anti-
Answer 180 DEG C/12h.The sample that hydro-thermal reaction is terminated carries out multiple filtering and washing, freeze-drying, then in the pipe of argon gas protection
800 DEG C of heat preservation 1h are warming up to the heating rate of 25 DEG C/min in formula furnace, the flow velocity of argon gas is in heat treatment process
500sccm。
(2) it etches transition metal material: heat-treated products is dissolved in stirring etching 1 day in the dilute hydrochloric acid of the 3M of 20ml,
Then filtering and washing product and dry to get arriving nitrogen sulphur codope porous graphene.
Embodiment 7
(1) it disperses 0.05g graphene oxide in the mixed solution of 80ml deionized water and 10ml ethyl alcohol, then successively
0.5g melamine, 0.75g trithiocyanuric acid and 1.5g cobalt nitrate hexahydrate is added, continues to stir under conditions of 120 DEG C
12min.Then the solution being transferred in polytetrafluoroethyllining lining and carries out hydro-thermal reaction, the packing ratio of hydro-thermal reaction is 40%,
80 DEG C/18h of hydro-thermal reaction.The sample that hydro-thermal reaction is terminated carries out multiple filtering and washing, then freeze-drying is protected in argon gas
Tube furnace in 400 DEG C of heat preservation 4h are warming up to the heating rate of 21 DEG C/min, the flow velocity of argon gas is in heat treatment process
500sccm。
(2) it etches transition metal material: heat-treated products is dissolved in stirring etching 1 day in the dilute hydrochloric acid of the 3M of 20ml,
Then filtering and washing product and dry to get arriving nitrogen sulphur codope porous graphene.
Embodiment 8
(1) it disperses 0.05g graphene oxide in the mixed solution of 60ml deionized water and 15ml ethyl alcohol, then successively
0.2g melamine, 0.05g trithiocyanuric acid and 1.5g cobalt nitrate hexahydrate is added, continues to stir under conditions of 60 DEG C
180min.Then the solution being transferred in polytetrafluoroethyllining lining and carries out hydro-thermal reaction, the packing ratio of hydro-thermal reaction is 85%,
80 DEG C/18h of hydro-thermal reaction.The sample that hydro-thermal reaction is terminated carries out multiple filtering and washing, then freeze-drying is protected in argon gas
Tube furnace in 400 DEG C of heat preservation 4h are warming up to the heating rate of 21 DEG C/min, the flow velocity of argon gas is in heat treatment process
500sccm。
(2) it etches transition metal material: heat-treated products is dissolved in stirring etching 1 day in the dilute hydrochloric acid of the 3M of 20ml,
Then filtering and washing product and dry to get arriving nitrogen sulphur codope porous graphene.
Finally it should be noted that: the above examples are only used to illustrate the technical scheme of the present invention rather than its limitations, to the greatest extent
Pipe is described the invention in detail referring to above-described embodiment, it should be understood by those ordinary skilled in the art that: still may be used
With modifications or equivalent substitutions are made to specific embodiments of the invention, and repaired without departing from any of spirit and scope of the invention
Change or equivalent replacement, should all cover in present claims range.
Claims (9)
1. a kind of preparation method of nitrogen sulphur codope porous graphene, it is characterised in that the following steps are included:
(1) by graphene oxide, melamine, trithiocyanuric acid and transition metal nitrate be successively scattered in ethyl alcohol and go from
In the mixed solution of sub- water, it is stirred to react sufficiently；The graphene oxide, melamine, trithiocyanuric acid, transition metal nitric acid
The mass ratio of salt is 1:(1.2~10): (1~15): (10~30)；The volume ratio of the middle ethyl alcohol and deionized water be 1:(1~
8)；
Then stirring product is transferred in water heating kettle and carries out hydro-thermal reaction；The time of the hydro-thermal reaction is 8-48h, hydro-thermal temperature
Degree is 80~200 DEG C；
(2) sample that hydro-thermal reaction terminates with deionized water filtering and washing for several times, then dry, dry sample be placed in inertia
Calcination processing is carried out in the tube furnace of gas shield；
In the calcination process, heating rate be 10~30 DEG C/min, holding temperature be 400~1000 DEG C, soaking time be 0~
4h；
(3) transition metal material in heat-treated products is etched away with dilute hydrochloric acid, then filtering and washing product and dry to get arriving
Nitrogen sulphur codope porous graphene.
2. the preparation method of nitrogen sulphur codope porous graphene according to claim 1, it is characterised in that: the step 1)
The time being stirred to react is 0.1~2h, and whipping temp is 50~140 DEG C.
3. the preparation method of nitrogen sulphur codope porous graphene according to claim 1, it is characterised in that: the step 1)
Middle transition metal nitrate is one of Nickelous nitrate hexahydrate, cabaltous nitrate hexahydrate and Fe(NO3)39H2O or a variety of.
4. the preparation method of nitrogen sulphur codope porous graphene according to claim 1, it is characterised in that: the step 1)
The packing ratio of middle hydro-thermal reaction is 40%~85%.
5. the preparation method of nitrogen sulphur codope porous graphene according to claim 1, it is characterised in that: the step 2)
In heat treatment, in the calcination process, the flow velocity of protective gas is 0-500sccm.
6. the preparation method of nitrogen sulphur codope porous graphene according to claim 1, it is characterised in that: the step 3)
Using the dilute hydrochloric acid of 0.5~5M when middle dilute hydrochloric acid etches, etch 1-5 days.
7. a kind of nitrogen sulphur codope porous graphene of the method preparation of any one according to claim 1~6.
8. nitrogen sulphur codope porous graphene according to claim 7, it is characterised in that: nitrogen atom doping amount is 2at%
~10at%, sulphur atom doping are 0.2at%~3at%, and mesoporous pore volume is 0.025-0.09cm3/g。
9. a kind of nitrogen sulphur codope porous graphene according to any one of claims 8 is negative as cathode of lithium battery active material, sode cell
Pole active material or lithium-sulfur cell carry the application of sulfur-donor.
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Application publication date: 20190621 |