CN110148531A - A kind of combination electrode material preparation method of carbon-based nitrogen sulphur codope - Google Patents
A kind of combination electrode material preparation method of carbon-based nitrogen sulphur codope Download PDFInfo
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- CN110148531A CN110148531A CN201910458702.7A CN201910458702A CN110148531A CN 110148531 A CN110148531 A CN 110148531A CN 201910458702 A CN201910458702 A CN 201910458702A CN 110148531 A CN110148531 A CN 110148531A
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- graphene
- thiocarbamide
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
Type of the present invention discloses a kind of graphene nanometer sheet, using thiocarbamide as dopant, prepares nitrogen, sulphur codope graphene using hydrothermal synthesis method.The graphene of acquisition has the characteristics that transparent, few layer structure.Graphene electrodes material preparation method, comprising: (1) prepare GO as presoma in the method that immersion method and chemical reaction combine.(2) certain density GO solution, ultrasound removing are configured.(3) certain mass thiocarbamide will be added in certain density GO solution and is used as dopant, and prepare to be put into autoclave after solution and carry out hydro-thermal reaction, preparation N, S codope graphene.The present invention, by changing experiment parameter, has prepared the superior graphene combination electrode material of capacitive property based on hydro-thermal method and chemical reaction.
Description
Technical field
The present invention relates to a kind of combination electrode material preparation methods of carbon-based nitrogen sulfur doping.
Background technique
2004, Univ Manchester UK physicist An Deliehaimu and Constantine's Nuo Woxiao love, at
Graphene is isolated to function from graphite in an experiment, and confirms that it can be with individualism, two people are also because " in two-dimensional graphene material
The initiative of material is tested " and Nobel Prize in physics in 2010 is obtained jointly.Graphene appear in scientific circles evoked it is huge
Great waves, correlative study paper sharply increases, the new potentiality as " the rear silicon epoch " for forming nanometer size transistor and circuit
Material, it is intended to also be sharply increased in the world using the research and development of graphene, the research of the country such as the U.S., South Korea, China is outstanding
It is active.Graphene or will become can be achieved high speed transistor, high sensor, laser, touch panel, battery and
The core material of a variety of devices of new generation such as high performance solar batteries, in recent years application of the graphene in supercapacitor are ground
Study carefully and has become a research hotspot.
Since there are lone pair electrons for sulphur and nitrogen-atoms, introduce them into carbon-based material, it can be with sp2Pi bond in hydridization C
Effect, improves the electric conductivity of carbon material, and generate fake capacitance, while having an impact to the specific surface area and structure of carbon material, from
And improve the specific capacitance of carbon material.The inner surface that Huang etc. makes it into active carbon by being heat-treated pure sheet sulphur obtains sulphur
Modification activities charcoal (SAC), SAC electrode show preferable electric conductivity, are 1.4 Ag in organic electrolysis plastidome current density-1
When, specific capacitance specific activity charcoal (AC) electrode height nearly 40%.Be covered on the surface AC sulfur-bearing functional group can with inhibitory activity material with have
The generation of the side reaction of machine electrolyte, to achieve the purpose that improve capacitive property.Thiophenecarboxaldehyde and the resorcinol such as Zhou
Freeze thousand gels by carbon of the sol-gel process synthesis rich in sulphur, exists as the increase of sulfur content can effectively improve carbon electrode
Wetability in organic electrolyte.Lee etc. introduces sulphur atom using a kind of mechanism of new generation fake capacitance in graphene,
Under the auxiliary of extrinsic current, the graphene airsetting of sulfur functionalization is obtained by the redox machinery between carbothioic acid ester and sulfo group
Glue is 1Ag in current density-1When, specific capacitance is up to 1089Fg-1Even if in 50Ag-1High current density under, than
Capacitor is also maintained at 833Fg-1, meanwhile, which has 43Whkg-1Energy density and 38Whkg-1Power it is close
Degree.This patent carries out Heteroatom doping to grapheme material surface using hydro-thermal method and is modified using thiocarbamide as dopant.Study N, S
It is co-doped with the influence to grapheme material object phase, microstructure and chemical property.And probe into dopant content, hydrothermal temperature and water
Influence of the hot time to grapheme material chemical property, the application that patent is graphene in supercapacitor provide theory
It is supported with data.
Summary of the invention
A kind of nitrogen, sulphur codope graphene nanometer sheet, it is characterised in that: with cotton-shaped graphite oxide (GO) for presoma,
Using thiocarbamide as dopant, nitrogen, sulphur codope graphene are prepared using hydrothermal synthesis method, acquisition is transparent, few layer structure
Graphene electrodes material, is compared with other methods, the graphene sample of nitrogen, sulphur codope, and under low sweep speed, CV curve is all
Good rectangle is kept, there is preferable electric double layer capacitance performance, the capacitive property of NGs sample is better than undoped after N doping.
The graphene nanometer sheet of acquisition has biggish aperture and biggish specific surface area, has higher conductivity, as supercapacitor
Electrode material there is outstanding chemical property and cyclical stability, the process for preparing graphene with this method is simple, safety.
The present invention provides a kind of preparation methods of graphene, comprising the following steps: step S1: using graphite, sodium nitrate,
The concentrated sulfuric acid waits chemicals, by chemical reaction, obtains cotton-shaped graphite oxide (GO) presoma；Step S2: GO is passed through super
The method of sound is removed form graphene oxide in deionized water；Step S3: graphene (RGO) is prepared using hydro-thermal method.
Further, the preparation method of the graphene, it is characterised in that: in the step S1, take 2g graphite, 1.5g nitre
Sour sodium measures the 80ml concentrated sulfuric acid, three is uniformly mixed in the beaker of 500ml, under condition of ice bath after magnetic agitation 20min
Slowly divide and 8g KMnO is added several times4, continue to stir 90min；Then beaker is transferred under 40 DEG C of water bath conditions and continues to stir
120ml deionized water is slowly added dropwise into solution by 90min, is added after continuing magnetic agitation 60min after then heating to 80 DEG C
15ml hydrogenperoxide steam generator by eccentric cleaning, freeze-drying, obtains cotton-shaped GO presoma after reaction.
Further, the preparation method of the graphene, it is characterised in that: in the step S2, weigh 0.05 g and make
Graphite oxide (GO) be dissolved in 50 ml deionized waters, after 30 min of magnetic agitation, 30 min of re-ultrasonic dispersion is formed uniform
GO dispersion liquid, then weigh a certain amount of thiocarbamide in mass ratio for 1:20 and be added in above-mentioned dispersion liquid, all dissolved to thiocarbamide
Afterwards, mixed solution is transferred in the water heating kettle that liner is polytetrafluoroethylene (PTFE).
Further, the preparation method of the graphene, it is characterised in that: in the step S3, then water heating kettle sealed
It is put into baking oven, is reacted under the conditions of 180 DEG C for 24 hours, after reaction cooled to room temperature, it is clear through deionized water to take out sample
It washes, be freeze-dried and obtain nitrogen, sulphur codope graphene, later, change mass ratio (1:0,1:20, the 1:60 of GO and thiocarbamide respectively
And 1:100), N, S codope graphene are prepared using reaction condition same as described above, gained sample is respectively labeled as RGO,
NS1-G, NS3-G and NS5-G.
After above-mentioned technical proposal, the invention has the following advantages: 1) graphene prepared by the present invention has
Better electric conductivity, capacitive property, the electrode material as supercapacitor have outstanding cyclical stability；2) present invention adopts
Graphene is prepared with immersion method and hydro-thermal method, raw material are easy to get, and cost is relatively low, and experimentation is simple.
Detailed description of the invention
Fig. 1 is the field emission scanning electron microscope photo of composite material of the present invention；Fig. 2 is composite wood feed powder of the invention
The XRD of body schemes.
Specific embodiment
In order that the present invention can be more clearly and readily understood, right below according to specific embodiment and in conjunction with attached drawing
The present invention is described in further detail.
Embodiment one:
A kind of graphene observes its pattern by scanning electron microscope.Fig. 1 is RGO, NS1-G, NS3-G and NS5-G sample
SEM figure.It can be seen from the figure that mutual unordered stacking between RGO sample lamella, forms 3D network structure, excess-three sample
Product then have similar pattern, structure that all show certain transparency, few layer and are formed in hydrothermal reaction process
Intrinsic fold, it is consistent with being reported in document；Fig. 2 is nitrogen, sulphur codope front and back gained RGO, NS1-G, NS3-G and NS5-G sample
The XRD diagram of product.It can be seen from the figure that nearby having a diffraction maximum in 2 θ=12.3 °, which is the characteristic peak of GO, is adulterated with N, S
The intensity of the increase of amount, this peak is gradually weakening, and especially in NS5-G sample, the peak is substantially unobvious.This show with
N, the increase of S doping, the degree that the oxygen-containing functional group of graphene surface is reduced increase, the oxygen-containing function in NS5-G sample
The amount of group is minimum.In the diffraction maximum that the diffraction maximum that 2 θ=24.8 ° occur is graphite (002) crystal face, there is a steamed bun in 2 θ=42.6 °
Diffraction maximum corresponds to (100) crystal face of graphite, and the diffraction maximum is very unobvious.According to above-mentioned analysis, after hydro-thermal method restores,
RGO and NSGs sample all forms the graphene-structured of fewer layers, but there are also the unreduced oxygen-containing functional groups in part in sample
In the presence of especially RGO sample.
Embodiment two:
The present invention provides a kind of preparation methods of graphene, comprising the following steps: step S1: utilizing graphite, sodium nitrate, dense sulphur
Acid waits chemicals, by chemical reaction, obtains cotton-shaped graphite oxide (GO) presoma；Step S2: GO is passed through into ultrasound
Method is removed form graphene oxide in deionized water；Step S3: graphene (RGO) is prepared using hydro-thermal method.
Preferably, the preparation method of the graphene, it is characterised in that: in the step S1, take 2g graphite, 1.5g nitre
Sour sodium measures the 80ml concentrated sulfuric acid, three is uniformly mixed in the beaker of 500ml, under condition of ice bath after magnetic agitation 20min
Slowly divide and 8g KMnO is added several times4, continue to stir 90min；Then beaker is transferred under 40 DEG C of water bath conditions and continues to stir
120ml deionized water is slowly added dropwise into solution by 90min, is added after continuing magnetic agitation 60min after then heating to 80 DEG C
15ml hydrogenperoxide steam generator by eccentric cleaning, freeze-drying, obtains cotton-shaped GO presoma after reaction.
Preferably, the preparation method of the graphene, it is characterised in that: in the step S2, weigh 0.05 g and make
Graphite oxide (GO) be dissolved in 50 ml deionized waters, after 30 min of magnetic agitation, 30 min of re-ultrasonic dispersion is formed uniform
GO dispersion liquid, then weigh a certain amount of thiocarbamide in mass ratio for 1:20 and be added in above-mentioned dispersion liquid, all dissolved to thiocarbamide
Afterwards, mixed solution is transferred in the water heating kettle that liner is polytetrafluoroethylene (PTFE).
Preferably, the preparation method of the graphene, it is characterised in that: in the step S3, then water heating kettle sealed
It is put into baking oven, is reacted under the conditions of 180 DEG C for 24 hours, after reaction cooled to room temperature, it is clear through deionized water to take out sample
It washes, be freeze-dried and obtain nitrogen, sulphur codope graphene, later, change mass ratio (1:0,1:20, the 1:60 of GO and thiocarbamide respectively
And 1:100), N, S codope graphene are prepared using reaction condition same as described above, gained sample is respectively labeled as RGO,
NS1-G, NS3-G and NS5-G.
For the present invention to utilize graphite, sodium nitrate, the concentrated sulfuric acid, waiting chemicals is raw material, passes through chemistry with immersion method first
Reaction, obtains cotton-shaped graphite oxide (GO) presoma.With cotton-shaped graphite oxide (GO) for presoma, then pass through hydro-thermal method,
The graphene nanometer sheet prepared has preferable electric conductivity, higher capacitive property, has outstanding follow as electrode material
Ring stability, the preparation process of graphene is simple, safe in the method.
Particular embodiments described above, pair present invention solves the technical problem that, technical scheme and beneficial effects carry out
It is further described, it should be understood that the above is only a specific embodiment of the present invention, is not limited to this
Invention, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be included in this hair
Within bright protection scope.
Claims (5)
1. a kind of nitrogen-doped graphene nanometer sheet, it is characterised in that: with cotton-shaped graphite oxide (GO) for presoma, made with thiocarbamide
For dopant, nitrogen, sulphur codope graphene are prepared using hydrothermal synthesis method, acquisition is transparent, layer structure less graphene electricity
Pole material, is compared with other methods, the graphene sample of nitrogen, sulphur codope, and under low sweep speed, CV curve all keeps good
Rectangle, have preferable electric double layer capacitance performance, N, S doping after sample capacitive property be better than undoped, the stone of acquisition
Black alkene nanometer sheet has biggish aperture and biggish specific surface area, there is higher conductivity, the electrode material as supercapacitor
Material has outstanding chemical property and cyclical stability, and the process for preparing graphene with this method is simple, safe.
2. the preparation method of graphene according to claim 1, comprising the following steps: step S1: utilizing graphite, nitric acid
Sodium, the concentrated sulfuric acid wait chemicals, by chemical reaction, obtain cotton-shaped graphite oxide (GO) presoma；Step S2: GO is led to
The method for crossing ultrasound is removed in deionized water forms graphene oxide；Step S3: graphene (RGO) is prepared using hydro-thermal method.
3. the preparation method of graphene according to claim 2, it is characterised in that: in the step S1, take 2g graphite,
1.5g sodium nitrate measures the 80ml concentrated sulfuric acid, three is uniformly mixed in the beaker of 500ml, the magnetic agitation under condition of ice bath
Slowly divide addition 8g KMnO several times after 20min4, continue to stir 90min；Then by beaker be transferred under 40 DEG C of water bath conditions after
Continuous stirring 90min, 120ml deionized water is slowly added dropwise into solution, after continuing magnetic agitation 60min after then heating to 80 DEG C
15ml hydrogenperoxide steam generator is added, after reaction, by eccentric cleaning, freeze-drying, obtains cotton-shaped GO presoma.
4. the preparation method of graphene according to claim 2, it is characterised in that: in the step S2, weigh 0.05 g
The graphite oxide (GO) made is dissolved in 50 ml deionized waters, and after 30 min of magnetic agitation, 30 min of re-ultrasonic dispersion is formed
Then uniform GO dispersion liquid weighs a certain amount of thiocarbamide in mass ratio for 1:20 and is added in above-mentioned dispersion liquid, to thiocarbamide whole
After dissolution, mixed solution is transferred in the water heating kettle that liner is polytetrafluoroethylene (PTFE).
5. the preparation method of graphene fiber according to claim 2, it is characterised in that: in the step S3, then by water
Hot kettle sealing is put into baking oven, is reacted under the conditions of 180 DEG C for 24 hours, after reaction cooled to room temperature, takes out sample through going
Ionized water cleaning, freeze-drying obtain nitrogen, sulphur codope graphene, later, change respectively GO and thiocarbamide mass ratio (1:0,1:
20,1:60 and 1:100), N, S codope graphene are prepared using reaction condition same as described above, gained sample marks respectively
For RGO, NS1-G, NS3-G and NS5-G.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111223688A (en) * | 2020-01-13 | 2020-06-02 | 北京化工大学 | Preparation method of nitrogen and sulfur co-doped graphene fiber supercapacitor electrode material |
| CN111999358A (en) * | 2020-08-17 | 2020-11-27 | 合肥工业大学 | Application of graphite-like phase carbon nitride nano material as electrochemical modified electrode material in methyl mercury detection |
| CN113559724A (en) * | 2021-07-12 | 2021-10-29 | 太原理工大学 | Preparation method and application of nitrogen and sulfur co-doped porous carbon sphere mixed matrix membrane |
| CN113957478A (en) * | 2021-11-11 | 2022-01-21 | 山西大学 | Sulfur and nitrogen co-doped graphene rich in edge defects and preparation method and application thereof |
| CN115472440A (en) * | 2022-08-18 | 2022-12-13 | 兰州大学 | Graphene-based N, S doped electrode material and preparation method thereof |
-
2019
- 2019-05-29 CN CN201910458702.7A patent/CN110148531A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111223688A (en) * | 2020-01-13 | 2020-06-02 | 北京化工大学 | Preparation method of nitrogen and sulfur co-doped graphene fiber supercapacitor electrode material |
| CN111999358A (en) * | 2020-08-17 | 2020-11-27 | 合肥工业大学 | Application of graphite-like phase carbon nitride nano material as electrochemical modified electrode material in methyl mercury detection |
| CN113559724A (en) * | 2021-07-12 | 2021-10-29 | 太原理工大学 | Preparation method and application of nitrogen and sulfur co-doped porous carbon sphere mixed matrix membrane |
| CN113559724B (en) * | 2021-07-12 | 2023-11-24 | 太原理工大学 | Preparation method and application of nitrogen-sulfur co-doped porous carbon sphere mixed matrix membrane |
| CN113957478A (en) * | 2021-11-11 | 2022-01-21 | 山西大学 | Sulfur and nitrogen co-doped graphene rich in edge defects and preparation method and application thereof |
| CN113957478B (en) * | 2021-11-11 | 2023-09-22 | 山西大学 | Sulfur and nitrogen co-doped graphene rich in edge defects, and preparation method and application thereof |
| CN115472440A (en) * | 2022-08-18 | 2022-12-13 | 兰州大学 | Graphene-based N, S doped electrode material and preparation method thereof |
| CN115472440B (en) * | 2022-08-18 | 2024-03-15 | 兰州大学 | Graphene-based N, S doped electrode material and preparation method thereof |
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