CN108975308A - A kind of level duct charcoal nanometer sheet and its preparation method and application - Google Patents
A kind of level duct charcoal nanometer sheet and its preparation method and application Download PDFInfo
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- CN108975308A CN108975308A CN201810896653.0A CN201810896653A CN108975308A CN 108975308 A CN108975308 A CN 108975308A CN 201810896653 A CN201810896653 A CN 201810896653A CN 108975308 A CN108975308 A CN 108975308A
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- nanometer sheet
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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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
A kind of level duct charcoal nanometer sheet and its preparation method and application, under room temperature, charcoal source, metal salt and sodium chloride mixing are added in distilled water, and magnetic agitation is completely dissolved charcoal source and metal salt, subsequent solvent evaporated;Gained sample is placed in tube furnace, is gradually heated to activation temperature under nitrogen protection, is passed through activating reagent, and activation a period of time at this temperature, then is cooled to room temperature under nitrogen atmosphere;Black solid successively uses distilled water, acid solution, distillation water washing, until metal salt-free and NaCl, up to level duct charcoal nanometer sheet after drying.Obtained material has level pore distribution, and thickness is adjustable in nanoscale, with excellent high rate performance when as electrode material for super capacitor.
Description
Technical field
The invention belongs to technical field of carbon material preparation, and in particular to a kind of level duct charcoal nanometer sheet and preparation method thereof
And application.
Background technique
Porous carbon material because have chemical property stabilization, large specific surface area, pattern and aperture controllable, it is low in cost with
And advantages of environment protection and be concerned by people, be widely used in energy storage, environmental protection, petrochemical industry, life
The fields such as object pharmacy and food industry.
Cellular structure and pore-size distribution are one of the key factors for influencing porous carbon material application performance.Level duct raw material of wood-charcoal
The characteristics of material is with macropore frame, mesoporous channels and micropore texture structure.In general, the macropore of porous carbon material can be made
For the buffer area of solution or ion, mesoporous then provides specific surface area and reacting environment as ion transmission channel, micropore.Because of tool
There are these features, level duct Carbon Materials become the focus of people's research, and especially store in supercapacitor electrochemical energy
Field.The level cellular structure of Carbon Materials is generally obtained by classification activation method, which needs to convert different activation examinations
Agent has the problems such as severe reaction conditions, complex process, larger environmental pollution hidden danger, limits answering for such Carbon Materials future
With and development.In addition it is also possible to level duct Carbon Materials are prepared by template, however this method needs expensive template
Agent, the removal of hard template generally require the hydrofluoric acid of strong corrosive, complex process and with high costs, it is difficult to scale application.
Pattern is another key factor for influencing porous carbon material application performance.Charcoal nanometer sheet is one kind with a thickness of nanoscale
Two-dimentional Carbon Materials because have high surface-to-volume ratio, good electric conductivity, controllable lamellar spacing and opening
Pore structure and be valued by people.The method for preparing charcoal nanometer sheet mainly includes mechanical stripping method, template, self-assembly method
With chemical vapour deposition technique etc..The generally existing complex process of these methods is time-consuming, it is at high cost, easily pollute the environment etc. and to lack
It falls into.
Supercapacitor is that one kind is big with power density, the charging time is fast, long service life, good temp characteristic, green
Environmental protection and the safe green energy-storing element of use.Carbon Materials are the most commonly used electrode material for super capacitor.Level duct charcoal
The macropore of material can be used as ion buffer area, mesoporous to be conducive to ion transmission, and micropore then optimizes charge storage, with
Its for electrode material supercapacitor often specific capacitance with higher and excellent high rate performance.Charcoal nanometer sheet has huge
Surface volume ratio, the contact area with electrolyte can be improved, shorten the diffusion path of electrolyte, while can also provide continuous
Electrical conductance path and strain relaxation, and a kind of excellent electrode material for super capacitor.However, in general level hole
Road Carbon Materials be often it is spherical or blocky, charcoal nanometer sheet then mostly based on micropore, the charcoal nanometer sheet with level cellular structure
Preparation method is also immature.Therefore, the level knot of a kind of simple process, large-scale production low in cost, environmentally protective, easy is found
The preparation method of structure charcoal nanometer sheet becomes current research tendency.
Summary of the invention
The technical issues of solution: the present invention provides a kind of preparation method and application of level duct charcoal nanometer sheet.With cheap
Sodium chloride be dispersing agent and template, metal salt be catalyst and occupy-place reagent, water-soluble biological matter be charcoal source, pyrolysis activation
And remove template and occupy-place reagent obtains the charcoal nanometer sheet with level cellular structure.
The preparation method of level duct charcoal nanometer sheet, this method have simple process, low in cost, environmentally protective and easy rule
The characteristics of modelling produces.Charcoal charcoal nanometer sheet is prepared with level pore distribution by this method, and thickness is adjustable in nanoscale, is used as
With excellent high rate performance when electrode material for super capacitor.
Technical solution: a kind of preparation method of level duct charcoal nanometer sheet, step includes: charcoal source, metal salt and sodium chloride
Mixing is added in distilled water, and the mass ratio in the charcoal source, metal salt and sodium chloride is 1:(0.2 ~ 0.6): (3 ~ 5), sodium chloride
Mass ratio with distilled water is 1:(1 ~ 3), room temperature magnetic agitation makes it completely dissolved, subsequent solvent evaporated;Gained sample is placed in
In tube furnace, 600 ~ 750 DEG C of activation temperature are gradually heated under nitrogen protection, heating rate is 1 ~ 10 DEG C/min, is passed through work
Change reagent, and activates 2 ~ 6 h under activation temperature, then be cooled to room temperature under nitrogen atmosphere and obtain black solid;Gained black solid
Distilled water, acid solution, distillation water washing are successively used, until metal salt-free and NaCl, up to layer after 100 ~ 300 DEG C of dryings
Grade duct charcoal nanometer sheet.
Preferably, above-mentioned charcoal source is glucose, fructose, sucrose, sodium lignin sulfonate or chitosan.
Preferably, above-mentioned metal salt is Fe (NO3)3·9H2O、FeCl3·6H2O、Fe(CH3COO)2、Ni(NO3)2·6H2O
Or NiCl2·6H2O。
Preferably, the temperature that above-mentioned solvent is evaporated is room temperature ~ 100 DEG C.
Preferably, above-mentioned activating reagent is selected from CO2、H2O contains 5vt.%NH3Ar gas.
Preferably, above-mentioned acid solution is HCl, H2SO4Or HNO3。
Level duct charcoal nanometer sheet made from above-mentioned preparation method.
Above-mentioned level duct charcoal nanometer sheet is preparing the application in electrode material for super capacitor.
Key of the invention is to have planned as a whole the key of nanometer sheet technology of preparing and level duct charcoal technology of preparing, formed
It is formed on lamella while nanometer sheet by the occupy-place effect and catalytic action of metal (reducing activation energy and catalyzed graphitization)
The hole in level duct.
The utility model has the advantages that the preparation method of gained level duct charcoal nanometer sheet is simple, low in cost, environmentally protective, easy scale
Metaplasia produces;Obtained material has level pore distribution, and thickness is adjustable in nanoscale, when being used as electrode material for super capacitor
With excellent high rate performance.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of level duct charcoal nanometer sheet.Wherein A is the scanning electron microscope (SEM) photograph of embodiment 1, B is implementation
The scanning electron microscope (SEM) photograph of example 3, the scanning electron microscope (SEM) photograph that C is embodiment 2.As shown, material prepared by embodiment 1 and embodiment 3
All in curly, illustrate that their lamellar spacing is very thin, material prepared by embodiment 2 does not crimp substantially, and lamella is thicker;It can
To infer, the thickness of nanometer sheet is related to the molecular size range in charcoal source, and the more big then thickness of molecular weight is bigger;Furthermore, it may also be seen that
Many holes not of uniform size.
Fig. 2 is the transmission electron microscope picture for the level duct charcoal nanometer sheet that embodiment 1 obtains.As shown, prepared material
Show bubble porous structure, it can be seen that remaining big mesoporous after apparent metal oxide removes, and the metal oxidation removed
Layer of charcoal around object is in onion shape, is typical graphitized charcoal structure.
Fig. 3 is the N for the level duct charcoal nanometer sheet that embodiment 1 obtains2Adsorption desorption curve.As shown, the N2Adsorption desorption etc.
Warm curve belongs to IV type thermoisopleth, shows the presence for having mesoporous;Hysteresis loop is H3 type, has jumping in high-voltage end adsorbance, is piece
Caused by the slit pore that the accumulation of shape ion generates, to further demonstrate the presence of nanometer sheet.
The graph of pore diameter distribution for the level duct charcoal nanometer sheet that the position Fig. 4 embodiment 1 obtains.As shown, material prepared
Aperture is distributed within the scope of 0 ~ 100 nm, it was demonstrated that its level cellular structure.
Fig. 5 is cyclic voltammetry curve figure of the Carbon Materials under different scanning speed.Wherein A is 1 gained level hole of embodiment
Cyclic voltammetry curve figure, the B of road charcoal nanometer sheet are merchandise active carbon cyclic voltammetry curve figure.As shown, with scanning speed
Increase, the cyclic voltammetry curve of 1 gained charcoal nanometer sheet of embodiment is still able to maintain rectangle, in contrast the circulation volt of normal activated carbon
Peace curve then gradually becomes olive shape by rectangle rapidly, illustrates that Carbon Materials prepared by the present invention have excellent high rate performance.
Fig. 6 is the charcoal nanometer sheet that different embodiments obtain and comparison merchandise active carbon under different charging and discharging currents density
Specific capacitance (ratio that Re is Carbon Materials capacitance at 20 A/g and under 1 A/g).As shown, prepare through the invention
The charge and discharge under high current of charcoal nanometer sheet are still able to maintain big specific capacitance, illustrate their excellent high rate performances.
Specific embodiment
Preferably to illustrate the present invention to reach the technical means and efficacy that predetermined goal of the invention is taken, below by tool
Body embodiment and attached drawing are illustrated.
Embodiment 1
At room temperature, 2 g sucrose, 0.8 g Fe (NO3)3·9H28 mL distilled water, magnetic are added in the mixture of O and 7.5 g NaCl
Solvent is evaporated off under the conditions of 40 DEG C after stirring 0.5 h in power, the sample after drying is placed in tube furnace, with 5 under nitrogen protection
DEG C/heating rate of min is warming up to 700 DEG C, it is subsequently passed containing 5vt.%NH3Ar gas, and 3 h are kept the temperature at 700 DEG C, from
So it is cooled to room temperature to obtain black foam shape solid.Black foam shape solid, which is washed with distilled water, removes NaCl, then 4 M's
4 h that flow back in HCl solution remove ferriferous oxide, and distillation water washing to pH is neutrality, are drying to obtain level duct charcoal at 100 DEG C
Nanometer sheet.
Embodiment 2
At room temperature, 1.2 g chitosan, 0.4 g Fe (NO3)3·9H210 mL distillation is added in the mixture of O and 5 g NaCl
Water and 2 mL glacial acetic acid are evaporated off solvent under the conditions of 80 DEG C after 12 h of magnetic agitation, the sample after drying are placed in tube furnace
In, 750 DEG C are warming up to the heating rate of 10 DEG C/min under nitrogen protection, is subsequently passed CO2, and 3 are kept the temperature at this temperature
H, cooled to room temperature.Black solid, which is washed with distilled water, removes NaCl, and 4 h that then flow back in the HCl of 4 M remove iron oxygen
Compound, distillation water washing to eluate pH are neutrality, dry level duct charcoal nanometer sheet at 150 DEG C.
Embodiment 3
At room temperature, 2 g glucose, 0.6 g Ni (NO3)3·6H210 mL distilled water are added in the mixture of O and 10 g NaCl,
Solvent is evaporated off under the conditions of 100 DEG C after 0.5 h of magnetic agitation, the sample after drying is placed in tube furnace, under nitrogen protection with
The heating rate of 5 DEG C/min is warming up to 750 DEG C, is subsequently passed containing 5vt.%NH3Ar gas, and 6 h are kept the temperature at 750 DEG C,
Naturally it is cooled to room temperature.Foaming solid, which is washed with distilled water, removes NaCl, then in the HNO of 4 M36 h that flow back in solution are removed
Ferriferous oxide, distillation water washing to pH are neutrality, are drying to obtain level duct charcoal nanometer sheet at 100 DEG C.
Technical solution of the present invention is described in detail in above-described embodiment, it should be understood that described above
Only presently preferred embodiments of the present invention is not intended to restrict the invention, any person skilled in the art, is not departing from this
Within the scope of inventive technique scheme, when the technology contents using the disclosure above make few modifications or be modified to equivalent variations etc.
Imitate embodiment, still, it is all done in spirit of the invention it is any modify or improve, should be included in model of the present invention
Within enclosing.
Claims (8)
1. a kind of preparation method of level duct charcoal nanometer sheet, it is characterised in that step includes: that charcoal source, metal salt and sodium chloride are mixed
Close and be added in distilled water, the mass ratio in the charcoal source, metal salt and sodium chloride is 1:(0.2 ~ 0.6): (3 ~ 5), sodium chloride with
The mass ratio of distilled water is 1:(1 ~ 3), room temperature magnetic agitation makes it completely dissolved, subsequent solvent evaporated;Gained sample is placed in pipe
In formula furnace, 600 ~ 750 DEG C of activation temperature are gradually heated under nitrogen protection, heating rate is 1 ~ 10 DEG C/min, is passed through activation
Reagent, and 2 ~ 6 h are activated under activation temperature, then be cooled to room temperature under nitrogen atmosphere and obtain black solid;Gained black solid according to
Secondary distilled water, acid solution, distillation water washing, until metal salt-free and NaCl, up to level after 100 ~ 300 DEG C of dryings
Duct charcoal nanometer sheet.
2. the preparation method of level duct charcoal nanometer sheet according to claim 1, it is characterised in that the charcoal source is grape
Sugar, fructose, sucrose, sodium lignin sulfonate or chitosan.
3. the preparation method of level duct charcoal nanometer sheet according to claim 1, it is characterised in that the metal salt is Fe
(NO3)3·9H2O、FeCl3·6H2O、Fe(CH3COO)2、Ni(NO3)2·6H2O or NiCl2·6H2O。
4. the preparation method of level duct charcoal nanometer sheet according to claim 1, it is characterised in that the temperature that the solvent is evaporated
Degree is room temperature ~ 100 DEG C.
5. the preparation method of level duct charcoal nanometer sheet according to claim 1, it is characterised in that the activating reagent is selected from
CO2、H2O contains 5vt.%NH3Ar gas.
6. the preparation method of level duct charcoal nanometer sheet according to claim 1, it is characterised in that the acid solution be HCl,
H2SO4Or HNO3。
7. level duct charcoal nanometer sheet made from any preparation method of claim 1-6.
8. level duct charcoal nanometer sheet described in claim 7 is preparing the application in electrode material for super capacitor.
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CN110015660A (en) * | 2018-11-19 | 2019-07-16 | 华南理工大学 | A kind of porous carbon nanosheet of Ag doping lignin and preparation method thereof and the application in electrode material for super capacitor |
CN110090639A (en) * | 2019-06-06 | 2019-08-06 | 河北工业大学 | The method of the one step preparation porous carbon supported catalyst of high dispersive type |
CN113299487A (en) * | 2021-05-24 | 2021-08-24 | 池州学院 | Composite electrode material and preparation method and application thereof |
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CN110090639A (en) * | 2019-06-06 | 2019-08-06 | 河北工业大学 | The method of the one step preparation porous carbon supported catalyst of high dispersive type |
CN113299487A (en) * | 2021-05-24 | 2021-08-24 | 池州学院 | Composite electrode material and preparation method and application thereof |
CN113299487B (en) * | 2021-05-24 | 2022-05-20 | 池州学院 | Composite electrode material and preparation method and application thereof |
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