CN108470890A - A kind of application of the preparation method of nitrogen sulphur codope three-dimensional grapheme, its product and the product that prepare - Google Patents
A kind of application of the preparation method of nitrogen sulphur codope three-dimensional grapheme, its product and the product that prepare Download PDFInfo
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- CN108470890A CN108470890A CN201810212106.6A CN201810212106A CN108470890A CN 108470890 A CN108470890 A CN 108470890A CN 201810212106 A CN201810212106 A CN 201810212106A CN 108470890 A CN108470890 A CN 108470890A
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- H01M10/00—Secondary cells; Manufacture thereof
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- 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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- 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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- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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Abstract
The present invention provides a kind of preparation method of nitrogen sulphur codope three-dimensional grapheme.Graphene oxide is scattered in deionization, graphene oxide dispersion is obtained, the ethanol solution of melamine powder and trithiocyanuric acid is then added, is fitted into after being uniformly dispersed in water heating kettle and carries out hydro-thermal reaction;Hydrothermal product is dried, is finally heat-treated.Application the present invention also provides the nitrogen sulphur codope three-dimensional grapheme and the graphene as electrode material.Product prepared by the present invention, nitrogen element content is 3 ~ 10%, and sulfur content is 0.5 ~ 3%.The invention has the advantages that experimental method is safe and non-toxic, and it is of low cost, it is easy to operate.Doping, three dimensional stress construction and redox graphene are realized using hydro-thermal method.Prepared doping three-dimensional grapheme large specific surface area, can be in lithium ion battery, the application of the fields such as ultracapacitor and electro-catalysis.
Description
Technical field
The present invention relates to carbon nanomaterial field, more particularly to a kind of preparation method of nitrogen sulphur codope three-dimensional grapheme,
The application of its product prepared and the product.
Background technology
The two dimensional crystal for the monoatomic layer thickness that graphene is made of carbon atom, the material with perfect structure of being known as
Material, because of its large specific surface area, conductivity is high, the big feature of intensity and be considered can be used as high lithium storage materials.However, experiment and reason
Prove bright, the active site of pure graphene is inadequate, does not have selectivity, does not have good matching degree in practical applications.It grinds
Study carefully and shows(Electrochimica Acta, 2016, 205:188-197.)Exotic atom doping can effectively solve answering for graphene
With problem, defect is introduced to provide active site.The doping method of exotic atom have CVD, epitaxial growth, arc discharge method, pyrolysis,
Hydro-thermal method, plasma method etc..And the methods of CVD, epitaxial growth are of high cost, experiment condition is harsh, it is difficult to realize extensive system
It is standby.In contrast, hydro-thermal method is at low cost, easy realization and can prepare uniform nano material and receive the favor of researcher.
Invention content
In order to overcome the above problem of the prior art, the purpose of the present invention is to provide a kind of nitrogen sulphur codope three-dimensional graphites
The preparation method of alkene, its application of the product and the product that prepare as electrode material.The method safety of the present invention is nontoxic, cost
It is cheap, it is easy to operate.The controllable nitrogen sulfur doping graphene large specific surface area of the doping of preparation, can be super in lithium ion battery
It applies in the fields such as capacitor and electro-catalysis.
In order to achieve the above objectives, present invention employs following technical schemes:
A kind of preparation method of nitrogen sulphur codope three-dimensional grapheme, specific steps include:
(1)Hydro-thermal reaction prepares precursor:Graphene oxide is scattered in deionized water first, obtains graphene oxide dispersion
Then liquid is added the ethanol solution of melamine powder and trithiocyanuric acid, is fitted into after stirring evenly in water heating kettle and carries out hydro-thermal
Reaction.After the completion of hydro-thermal reaction, freeze-drying obtains presoma.
(2)Heat treatment prepares three-dimensional doped graphene:Presoma is placed in tube furnace, argon gas protection is passed to and carries out hot place
Reason.
Preferably, the step(1)Middle graphene oxide, melamine, trithiocyanuric acid mass ratio be 1:0.3~
2.5:0.4~3.5。
Preferably, the step(1)A concentration of mg/ml of 4 mg/ml ~ 10 of middle graphene oxide dispersion.
Preferably, the step(1)Described in the volume ratio of deionized water and ethanol consumption be 1:1~2.5.
Preferably, the step(1)Middle whipping temp is 70 ~ 120 DEG C, and mixing time is 10 ~ 60 min.
Preferably, the step(1)The reaction temperature of middle hydro-thermal reaction is 120 ~ 200 DEG C, and the reaction time is 4 ~ 36 h.
Preferably, the step(1)The packing ratio of middle hydro-thermal reaction is the % of 35 % ~ 50.
Preferably, the step(1)The heating rate of middle heat treatment is 2 ~ 10 DEG C/min, and holding temperature is 600 ~ 1000
DEG C, soaking time is 1 ~ 5h.
Advantageous effect of the invention is embodied in:
The present invention is poly- and form carbon skeleton and support graphene using melamine and trithiocyanuric acid supermolecule, inhibit graphene because
The reunion that Van der Waals force and π-π are stacked.Meanwhile melamine and trithiocyanuric acid be as nitrogen source and sulphur source, in hydro-thermal reaction and
It is heat-treated in journey and realizes nitrogen element sulphur codope.The invention has the advantages that realizing that doping, three dimensional stress construct simultaneously using hydro-thermal method
And redox graphene.Its nitrogen element content is 3 ~ 7%, and for sulfur content 1 ~ 3%, doping is controllable;In addition, graphene
It can be automatically assembled into three-dimensional shape graphene in hydro-thermal reaction, possibility is provided for large specific surface area;Experimental method is safe and non-toxic,
It is of low cost, it is easy to operate.Prepared doping three-dimensional grapheme, can be in lithium ion battery, ultracapacitor and electro-catalysis
Equal fields application.Therefore method provided by the invention has broad application prospects.
Description of the drawings
Fig. 1 is the scanning electron microscopy of the nitrogen sulphur codope three-dimensional grapheme prepared by embodiment 2(SEM)Photo;
Fig. 2 is the X-ray energy spectrum of the nitrogen sulphur codope three-dimensional grapheme prepared by embodiment 2(XPS)Spectrogram;
Fig. 3 is cyclic voltammetric of the nitrogen sulphur codope three-dimensional grapheme as lithium ion battery negative material prepared by embodiment 2
Curve.
Specific implementation mode
The present invention is further elaborated With reference to embodiment, but the present invention is not limited to following implementation
Example.
Embodiment 1
(1)Hydro-thermal reaction prepares precursor:100mg graphene oxides are scattered in 10ml deionized waters first, are aoxidized
Graphene dispersing solution, is then added 0.03g melamines, and 80 DEG C of stirrings obtain A liquid to being completely dissolved;Separately take tri- polysulfides of 0.04g
Cyanic acid is dissolved in 25ml ethyl alcohol, after obtain B liquid;B liquid is slowly added in A liquid, is fitted into water heating kettle after 70 DEG C of stirring 10min,
Packing ratio is 35%, 120 DEG C/4h of hydro-thermal reaction.After the completion of hydro-thermal reaction, freeze-drying obtains presoma.
(2)Heat treatment prepares three-dimensional doped graphene:Presoma is placed in tube furnace, pass to argon gas protection, with 2 DEG C/
The heating rate of min is warming up to 600 DEG C of heat preservation 5h.
Embodiment 2
(1)Hydro-thermal reaction prepares precursor:100mg graphene oxides are scattered in 25ml deionized waters first, are aoxidized
Graphene dispersing solution, is then added 0.13g melamines, and 80 DEG C of stirrings obtain A liquid to being completely dissolved;Separately take tri- polysulfides of 0.18g
Cyanic acid is dissolved in 25ml ethyl alcohol, after obtain B liquid;B liquid is slowly added in A liquid, is fitted into water heating kettle after 80 DEG C of stirring 60min,
Packing ratio is 50%, 200 DEG C/12h of hydro-thermal reaction.After the completion of hydro-thermal reaction, freeze-drying obtains presoma.
(2)Heat treatment prepares three-dimensional doped graphene:Presoma is placed in tube furnace, pass to argon gas protection, with 5 DEG C/
The heating rate of min is warming up to 700 DEG C of heat preservation 2h.
Referring to Fig.1, Fig. 1 is the SEM photograph that the present embodiment prepares sample.Electricity is scanned with the S-4800 types of Japan Electronics Corporation
Sub- microscope(SEM)Morphology observation is carried out, can significantly be seen three-dimensional made of being assembled by the graphene of nanometer grade thickness
Graphene, short texture, nanometer sheet are apparent.
With reference to Fig. 2, using x-ray photoelectron spectroscopy(XPS)Illustrate the bonding state of doped chemical and carbon, it is quantitative to adulterate
The content of element.Fig. 2 is the xps energy spectrum that the present embodiment prepares sample.Wherein,(a)For the full spectrograms of XPS of sample,(b)For C's
XPS swarming collection of illustrative plates,(c)For the swarming collection of illustrative plates of the XPS of N,(d)For the XPS swarming collection of illustrative plates of S.The sample can be seen in full spectrogram (a)
There are nitrogen and element sulphur in product other than carbon and oxygen element, illustrates that nitrogen element sulphur has successfully been doped into graphene
In.
With reference to Fig. 3, Fig. 3 is the stable circulation linearity curve that the present embodiment prepares sample.By sample assembly at CR2032 type lithiums
Ion battery carries out charge-discharge test, is 100mAh g in current density-1The test loop stability that Shi Xunhuan 100 is enclosed., can
Be clearly seen that sample cycle 100 circle after capacity still close to 600mAh g-1, and it is with good stability.
Embodiment 3
(1)Hydro-thermal reaction prepares precursor:100mg graphene oxides are scattered in 20ml deionized waters first, are aoxidized
Graphene dispersing solution, is then added 0.252g melamines, and 120 DEG C of stirrings obtain A liquid to being completely dissolved;Separately take 0.354 trimerization
Thiocyanic acid is dissolved in 25ml ethyl alcohol, after obtain B liquid;B liquid is slowly added in A liquid, water heating kettle is packed into after 120 DEG C of stirring 10min
In, packing ratio 55%, 150 DEG C/36h of hydro-thermal reaction.After the completion of hydro-thermal reaction, freeze-drying obtains presoma.
(2)Heat treatment prepares three-dimensional doped graphene:Presoma is placed in tube furnace, pass to argon gas protection, with 10 DEG C/
The heating rate of min is warming up to 1000 DEG C of heat preservation 1h.
Embodiment 4
(1)Hydro-thermal reaction prepares precursor:100mg graphene oxides are scattered in 15ml deionized waters first, are aoxidized
Graphene dispersing solution, is then added 0.03g melamines, and 80 DEG C of stirrings obtain A liquid to being completely dissolved;Separately take tri- polysulfides of 0.09g
Cyanic acid is dissolved in 25ml ethyl alcohol, after obtain B liquid;B liquid is slowly added in A liquid, is fitted into water heating kettle after 80 DEG C of stirring 20min,
Packing ratio is 40%, 180 DEG C of hydro-thermal reaction/for 24 hours.After the completion of hydro-thermal reaction, vacuum drying obtains presoma.
(2)Heat treatment prepares three-dimensional doped graphene:Presoma is placed in tube furnace, pass to argon gas protection, with 5 DEG C/
The heating rate of min is warming up to 700 DEG C of heat preservation 3h.
Embodiment 5
(1)Hydro-thermal reaction prepares precursor:100mg graphene oxides are scattered in 20ml deionized waters first, are aoxidized
Graphene dispersing solution, is then added 0.126 melamine, and 80 DEG C of stirrings obtain A liquid to being completely dissolved;Separately take 0.177 3 polysulfides
Cyanic acid is dissolved in 25ml ethyl alcohol, after obtain B liquid;B liquid is slowly added in A liquid, is fitted into water heating kettle after 70 DEG C of stirring 60min,
Packing ratio is 45%, 200 DEG C/4h of hydro-thermal reaction.After the completion of hydro-thermal reaction, freeze-drying obtains presoma.
(2)Heat treatment prepares three-dimensional doped graphene:Presoma is placed in tube furnace, pass to argon gas protection, with 2 DEG C/
The heating rate of min is warming up to 900 DEG C of heat preservation 2h.
Embodiment 6
(1)Hydro-thermal reaction prepares precursor:100mg graphene oxides are scattered in 25ml deionized waters first, are aoxidized
Graphene dispersing solution, is then added 0.25g melamines, and 80 DEG C of stirrings obtain A liquid to being completely dissolved;Separately take tri- polysulfides of 0.35g
Cyanic acid is dissolved in 25ml ethyl alcohol, after obtain B liquid;B liquid is slowly added in A liquid, is fitted into water heating kettle after 120 DEG C of stirring 60min,
Packing ratio is 50%, 200 DEG C/36h of hydro-thermal reaction.After the completion of hydro-thermal reaction, freeze-drying obtains presoma.
(2)Heat treatment prepares three-dimensional doped graphene:Presoma is placed in tube furnace, pass to argon gas protection, with 10 DEG C/
The heating rate of min is warming up to 1000 DEG C of heat preservation 5h.
Claims (10)
1. a kind of preparation method of nitrogen sulphur codope three-dimensional grapheme, which is characterized in that include the following steps:
1)Hydro-thermal reaction prepares precursor:Graphene oxide is scattered in enough deionized waters, obtains graphene oxide point
Dispersion liquid, the ethanol solution that melamine powder then is added, trithiocyanuric acid is added, hydro-thermal reaction is carried out after stirring evenly;It will
Hydrothermal product is dried, and presoma is obtained;
2)Heat treatment prepares three-dimensional doped graphene:By step 1)The presoma of preparation under protection of argon gas, in 600 ~ 1000 DEG C
It is heat-treated.
2. a kind of preparation method of nitrogen sulphur codope three-dimensional grapheme according to claim 1, it is characterised in that:The oxygen
Graphite alkene, melamine, trithiocyanuric acid mass ratio be 1:0.3~2.5:0.4~3.5.
3. a kind of preparation method of nitrogen sulphur codope three-dimensional grapheme according to claim 1, it is characterised in that:The oxygen
It is 4mg/ml ~ 10mg/ml that graphite alkene, which is scattered in the dispersion liquid concentration obtained in deionized water,.
4. a kind of preparation method of nitrogen sulphur codope three-dimensional grapheme according to claim 1, it is characterised in that:It is described to go
The volume ratio of ionized water and ethanol consumption is 1:1~2.5.
5. a kind of preparation method of nitrogen sulphur codope three-dimensional grapheme according to claim 1, it is characterised in that:The step
Rapid 1)Whipping temp be 70 ~ 120 DEG C, mixing time be 10 ~ 60 min.
6. a kind of preparation method of nitrogen sulphur codope three-dimensional grapheme according to claim 1, it is characterised in that:The water
The reaction temperature of thermal response is 120 ~ 200 DEG C, and the reaction time is 4 ~ 36 h.
7. a kind of preparation method of nitrogen sulphur codope three-dimensional grapheme according to claim 1, it is characterised in that:The water
The packing ratio of thermal response is the % of 35 % ~ 50.
8. a kind of preparation method of nitrogen sulphur codope three-dimensional grapheme according to claim 1, it is characterised in that:The step
Rapid 2)In heat treatment, heat treatment temperature be 600 ~ 1000 DEG C, heat treatment time be 1 ~ 5h.
9. the nitrogen sulphur codope three-dimensional grapheme prepared by any one of claim 1 ~ 8 method.
10. application of the nitrogen sulphur codope three-dimensional grapheme as electrode material described in claim 9.
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CN109244368A (en) * | 2018-11-19 | 2019-01-18 | 北京师范大学 | A kind of application of nitrogen-doped graphene in negative electrode of lithium ion battery preparation |
CN109485031A (en) * | 2018-11-19 | 2019-03-19 | 北京师范大学 | A kind of nitrogen-doped graphene and preparation method thereof |
CN109585185A (en) * | 2018-11-16 | 2019-04-05 | 郑州轻工业学院 | The confinement the preparation method and its stored energy application of a kind of nitrogen, sulphur codope graphene film |
CN109659546A (en) * | 2018-12-26 | 2019-04-19 | 成都爱敏特新能源技术有限公司 | A kind of sulphur/nitrogen/silicon coblended composite cathode material of silicon/carbon/graphite and preparation method thereof |
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