CN108492996A - A kind of preparation method of fluorine, nitrogen co-doped class graphene film layer material - Google Patents
A kind of preparation method of fluorine, nitrogen co-doped class graphene film layer material Download PDFInfo
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- CN108492996A CN108492996A CN201810177389.5A CN201810177389A CN108492996A CN 108492996 A CN108492996 A CN 108492996A CN 201810177389 A CN201810177389 A CN 201810177389A CN 108492996 A CN108492996 A CN 108492996A
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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
- 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
The invention discloses the preparation methods of a kind of fluorine, nitrogen co-doped class graphene film layer material, it is characterized in that, in the salt template of lithium chloride and potassium chloride mixing material, aminoglucose hydrochloride is mixed to simultaneously ball milling with polyvinylidene fluoride, then it is carbonized under an argon, it is washed by pickling, finally vacuum drying obtains fluorine, nitrogen co-doped class graphene film layer material.Fluorine, the nitrogen co-doped class graphene film layer material that the carbonization of one step of present invention salt template is prepared, wherein class graphene sheet layer is relatively thin, and fluorine, nitrogen are evenly distributed, good stability of the dimension, reproducible, fluorine nitrogen element content can regulate and control with polyvinylidene fluoride additive amount.Method is simple, and one-step synthesis, carburizing temperature is moderate, and fluorine, the nitrogen co-doped class graphene film layer material being prepared, specific discharge capacity is very high, and cyclical stability is fine, and electric conductivity is fine.The present invention above has good foreground in the application of ultracapacitor energy storage material.
Description
Technical field
It is the invention belongs to the preparation field that base metal codope carbon material is modified, more particularly to a kind of fluorine, nitrogen co-doped
Class graphene film layer material preparation method.
Background technology
With the rapid development of industry, population sharply increases, and the consumption of global energy just constantly adds with surprising rapidity
Soon, energy shortage and environmental pollution become current mankind and develop two test faced.Therefore must greatly develop low cost, can
Continue and environmental-friendly novel energy conversion and storage device are increasingly prominent come the growth requirement and alleviation for meeting modern society
The environmental problem gone out.Sustainable and environment friendly material is mentioned, people expect being exactly carbon material first.The source of carbon material
It is very abundant, it is inexhaustible, chemical contamination is small.Since 2004, Novoselov and Geim adhesive tapes were from block
The graphene that single layer has been separated in body graphite, to cause the largely research to graphene.
Graphene is stripped out from graphite material, and two dimension be made of carbon atom and only one layer atomic thickness is brilliant
Body.Graphene has many unique properties, including：Theoretical specific surface area is big, good conductivity, chemical stability and thermal stability
Good, potential windows mouth width and flexible etc..More than ten years get off, and the research temperature of grapheme material does not subtract, list truly
Atom layer graphene is difficult to be made, and the graphene that present people mention is the graphene of several lamellar spacings mostly.It is single at present
Grapheme material early has been unable to meet requirement of the people to material property, and in this more than ten years, people carry out grapheme material
Various modifications include the study on the modification of preparation method and material property.
Doping is a kind of common method of modifying, is adulterated from initial one-component, and nitrogen, boron, phosphorus, sulphur etc. carry out carbon material
It is modified, to multicomponent codope in recent years.Wherein N doping can inhibit oxygen content, reduce self discharge behavior and electronic contact
Resistance improves carbon surface wettability.Meanwhile the carbon of N doping is by wide coverage because the electronegativity (3.04) of nitrogen can induce
The Charge scaling of adjacent atom on nitrogen-doped carbon surface, this will greatly improve carbon electro-catalysis or generate faraday's reaction, contribution
Part fake capacitance.Although N doping can effectively improve the chemical property of carbon material, excessive nitrogen can lead to material itself
Resistance becomes larger, and nitrogen-containing functional group blocks duct, to reduce the electric conductivity of material.It is fluorine member that electronegativity is maximum in nature
Element, since big electronegativity is conducive to chemical property, researcher is natural it is also envisaged that being adulterated with fluorine element.So in recent years,
People have also carried out many fluorine, nitrogen co-doped research.The synergistic effect of fluorine and the nitrogen high electronegativity of its own and the two, greatly
The big chemical property for improving carbon material.Either there is larger carry to electrocatalysis characteristic or capacitance and stability
It rises.Fluorine is adulterated in carbon material and always needs a large amount of Fluorine source, will be extremely difficult in Fluorin doped to porous carbon matrix.Mesh
Before, ammonium fluoride is most common one kind.The easy decomposability of ammonium fluoride increases the synthesis difficulty of Fluorin doped porous carbon.Therefore, it opens
Sending out Fluorin doped method efficient has a very important significance.According to the pertinent literature of reference, Fluorine source be typically PVDF, PTFE,
NH4F。
Preparation method also there are many planting, such as low-temperature solvent heat method, is that carbon nitrogen three introduces a collections of fluorine are molten in organic solvent, is added
Then stabilizer reacts a few hours under hundreds of degrees Celsius.The carbon material degree of graphitization made in this way is not high, pore-creating and regulation and control ratio
Surface area is difficult.Also finished product grapheme material is immersed in fluorine nitrogen aqueous solution, by hydro-thermal reaction, nitrogen and fluorine are first in doping
Element, finished product graphene are prepared with the method for mechanical stripping, are difficult to accomplish homogeneity in size.
Invention content
Technical problem to be solved by the invention is to provide the preparations of a kind of fluorine, nitrogen co-doped class graphene film layer material
Method, the fluorine of preparation, nitrogen co-doped class graphene film layer material, lamella is relatively thin, and fluorine, N doping are evenly distributed.
To solve the above-mentioned problems, the present invention provides the preparations of a kind of fluorine, nitrogen co-doped class graphene film layer material
Method, which is characterized in that in the salt template of lithium chloride and potassium chloride mixing material, by aminoglucose hydrochloride and poly- inclined two
Vinyl fluoride mixing and ball milling, are then carbonized, are washed by pickling under an argon, and it is total to obtain fluorine, nitrogen for finally vacuum drying
Class graphene (FNC) sheet layer material of doping.
Preferably, the lithium chloride, potassium chloride, aminoglucose hydrochloride and polyvinylidene fluoride are powdered
Grain.
Preferably, the time of the ball milling is 0.5h.
Preferably, the carbonization carries out in argon atmosphere；The temperature of carbonization is 600 DEG C, and heating rate is 5 DEG C/min,
Soaking time is 2h.
Preferably, the pickling uses mass concentration to wash 8~12h for 5% dilute hydrochloric acid；Washing, which is adopted, to be washed with deionized water
Wash 8~12h.
Preferably, the vacuum drying is 60 DEG C of dry 12h in vacuum drying oven.
Fluorine, the nitrogen prepared the present invention also provides the preparation method of above-mentioned fluorine, nitrogen co-doped class graphene film layer material
Application of the class graphene film layer material of codope in the energy storage material of ultracapacitor.
Fluorine, the nitrogen co-doped class graphene film layer material that the carbonization of one step of present invention salt template is prepared, wherein
Class graphene sheet layer is relatively thin, and fluorine, nitrogen are evenly distributed, and good stability of the dimension is reproducible, and fluorine nitrogen element content can be with poly- inclined
Difluoroethylene (PVDF) additive amount regulates and controls.
The method of the present invention is simple, and one-step synthesis, carburizing temperature is moderate, fluorine, the nitrogen co-doped class graphene being prepared
Sheet layer material, specific discharge capacity is very high, and cyclical stability is fine, and electric conductivity is fine.It is relatively cheap as pure carbon material,
The application of ultracapacitor energy storage material above has good foreground.
Description of the drawings
Fig. 1 is the SEM figures of 10,000 times of FNC materials made from comparative example 1；
Fig. 2 a are the SEM figures of fluorine in embodiment 1, nitrogen co-doped class graphene film layer material FNC-1；
Fig. 2 b are the SEM figures of fluorine in comparative example 1, nitrogen co-doped class graphene film layer material FNC-2；
Fig. 2 c are the SEM figures of fluorine in comparative example 2, nitrogen co-doped class graphene film layer material FNC-3；
Fig. 3 is the XRD diagram of embodiment 1 and fluorine, nitrogen co-doped class graphene film layer material in comparative example 1, comparative example 2；
Fig. 4 is the XPS figures of comparative example 1 and fluorine, nitrogen co-doped class graphene film layer material in comparative example 1, comparative example 2；
Fig. 5 is the CV cycle figures of fluorine in embodiment 1, nitrogen co-doped class graphene film layer material；
Fig. 6 is the CV cycle figures of fluorine in comparative example 1, nitrogen co-doped class graphene film layer material；
Fig. 7 is the CV cycle figures of fluorine in comparative example 2, nitrogen co-doped class graphene film layer material；
Fig. 8 is embodiment 1 and fluorine, nitrogen co-doped class graphene film layer material 10mV/s speed in comparative example 1, comparative example 2
CV cycles figure under rate；
Fig. 9 is that the charge and discharge in embodiment 1 under fluorine, nitrogen co-doped class graphene film layer material difference current density are bent
Line；
Figure 10 is that the charge and discharge in comparative example 1 under fluorine, nitrogen co-doped class graphene film layer material difference current density are bent
Line；
Figure 11 is that the charge and discharge in comparative example 2 under fluorine, nitrogen co-doped class graphene film layer material difference current density are bent
Line；
Figure 12 is embodiment 1 and fluorine, nitrogen co-doped class graphene film layer material difference electric current in comparative example 1, comparative example 2
Capacity audio-visual picture under density；
Figure 13 is the electrochemistry of embodiment 1 and fluorine, nitrogen co-doped class graphene film layer material in comparative example 1, comparative example 2
Impedance diagram.
Specific implementation mode
In order to make the present invention more obvious and understandable, hereby with preferred embodiment, and attached drawing is coordinated to be described in detail below.
Embodiment 1
A kind of preparation method of fluorine, nitrogen co-doped class graphene film layer material：
(1) 0.02g polyvinylidene fluoride (PVDF) and 0.1g aminoglucose hydrochlorides are added to 10g (4.5g/5.5g)
After in lithium chloride/potassium chloride salt template, it is transferred to canister simultaneously and is sealed with sealed membrane.By container ball in the ball mill
Grind 30min, it is therefore an objective to allow block material ball to clay into power and four components are uniformly mixed.Then the powder after ball milling is transferred to
In the crucible of 50ml, under an argon, with the heating rate of 5 DEG C/min, rises to 600 DEG C and keep the temperature 2h, with 5% concentration after taking-up
Salt acid elution, deionized water wash each 8~12h, and fluorine, nitrogen co-doped class graphene film is made in last 60 DEG C of vacuum drying 12h
Layer material FNC-1.
(2) by fluorine, nitrogen co-doped class graphene film layer material FNC-1,20mg acetylene black, 10mg in 70mg steps (1)
10% concentration PVDF binders mixing, then use mortar grinder 30min, be subsequently added into 500 μ L N-methyls pyrrolidones (NMP)
Dilution, then the active material is applied on the carbon paper of known quality, last 60 DEG C of vacuum drying 6h weighs and calculates active material
Quality.
(3) the close carbon paper assembling electric double layer symmetric capacitor of two panels active mass, electrolyte is taken to select the hydrogen-oxygen of 6mol/L
Change potassium solution, its chemical property is tested with Shanghai Chen Hua electrochemical workstation.
Fig. 2 a show：Find out that the class graphene sheet layer of embodiment 1 is very thin from SEM figures, about tens nanometers of layer thickness, and point
Cloth is more uniform.
Fig. 5,12 show：From cyclic voltammetry curve find out FNC-1 have good cyclical stability, good specific capacity and
Outstanding high rate performance.
Comparative example 1
It is prepared according to the preparation method of embodiment 1, unlike, the dosage of the polyvinylidene fluoride (PVDF) is
Fluorine, nitrogen co-doped class graphene film layer material FNC-2 is made in 0.1g.
Fig. 2 b show：Find out that the class graphene sheet layer of comparative example 1 is very thin from SEM figures, about tens nanometers of layer thickness, slightly
It is thicker than example 1, but its distribution is more uniformly compared with example 1.
Fig. 6,12 show：Find out that FNC-2 has good cyclical stability from cyclic voltammetry curve, highest ratio in three
Capacity and outstanding high rate performance.
Comparative example 2
It is prepared according to the preparation method of embodiment 1, unlike, the dosage of the polyvinylidene fluoride (PVDF) is
Fluorine, nitrogen co-doped class graphene film layer material FNC-3 is made in 0.5g.
Fig. 2 c show：Find out that comparative example 2 does not have class graphene sheet layer structure from SEM figures, shows agraphitic carbon, pattern
Be particle clusters together.
Fig. 7,12 show：Find out that FNC-3's has good cyclical stability, good specific capacity from cyclic voltammetry curve
With poor high rate performance.
From Figure 2 it can be seen that finding out from SEM, as PVDF dosages increase, lamella becomes amorphous pellets again from thin thicken.It says
There are a limits for bright carbon and the amount ratio of salt template, will be unable to sheet layer material at preparation more than this limit.
As seen from Figure 3, can find out from XRD spectrum, two broad peaks correspond to agraphitic carbon and graphitic carbon, pass through the XRD
It reflects, pickling obtains very thorough, and salt template is all cleaned, and miscellaneous peak is not present.
From fig. 4, it can be seen that can find out from XPS collection of illustrative plates, fluorine, nitrogen content, and by the analysis to curve, with reference to phase
It closes document to be known that in the material there are the nitrogen of three kinds of forms i.e. pyridine nitrogen, pyrroles's nitrogen, graphite nitrogen, exists simultaneously C-F keys.This
Illustrating fluorine element, nitrogen, all successfully doping is entered.
As seen from Figure 8, the cyclic voltammetry curve under 10 mv s multiplying powers more acurrate can intuitively compare the big of capacity
It is small.In general the size of ring specific area corresponds to the size of capacity, from can find out that FNC-2 has most in comparative example 1 in the figure
Big ring specific area.
By Fig. 8 and Figure 12 as it can be seen that in three kinds of samples, FNC-2 has highest specific capacity and best high rate performance.This returns
Because in its class graphene sheet layer with suitable thickness, can be closely superimposed in stacking procedure, ensure that the stability of itself,
It is not easy to cave in charge and discharge process broken；At the same time the nitrogen co-doped amount of moderate fluorine allows it to have relatively high specific capacity.
As seen from Figure 13, the electric conductivity of material can be found out from impedance curve, the slope of curve is bigger, represents electric conductivity and gets over
It is good.General carbon material electric conductivity is related to degree of graphitization and carbon content, and three kinds of samples are carbonized at the same temperature, is graphitized journey
Degree is not much different, and how much electric conductivity size meets carbon source addition.
Claims (7)
1. the preparation method of a kind of fluorine, nitrogen co-doped class graphene film layer material, which is characterized in that in lithium chloride and potassium chloride
In the salt template of mixing material, aminoglucose hydrochloride is mixed to simultaneously ball milling with polyvinylidene fluoride, then in argon gas
It is carbonized under atmosphere, is washed by pickling, finally vacuum drying obtains fluorine, nitrogen co-doped class graphene film layer material.
2. the preparation method of fluorine as described in claim 1, nitrogen co-doped class graphene film layer material, which is characterized in that institute
It is powdery granule to state lithium chloride, potassium chloride, aminoglucose hydrochloride and polyvinylidene fluoride.
3. the preparation method of fluorine as described in claim 1, nitrogen co-doped class graphene film layer material, which is characterized in that institute
The time for stating ball milling is 0.5h.
4. the preparation method of fluorine as described in claim 1, nitrogen co-doped class graphene film layer material, which is characterized in that institute
Carbonization is stated to carry out in argon atmosphere；The temperature of carbonization is 600 DEG C, and heating rate is 5 DEG C/min, soaking time 2h.
5. the preparation method of fluorine as described in claim 1, nitrogen co-doped class graphene film layer material, which is characterized in that institute
Stating pickling uses mass concentration to wash 8~12h for 5% dilute hydrochloric acid；Washing, which is adopted, is washed with deionized 8~12h.
6. the preparation method of fluorine as described in claim 1, nitrogen co-doped class graphene film layer material, which is characterized in that institute
Vacuum drying is stated as 60 DEG C of dry 12h in vacuum drying oven.
7. the preparation method system of the fluorine, nitrogen co-doped class graphene film layer material described in a kind of claim 1-6 any one
Application of the standby fluorine, nitrogen co-doped class graphene film layer material in the energy storage material of ultracapacitor.
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Cited By (5)
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| CN109052367A (en) * | 2018-09-30 | 2018-12-21 | 华中科技大学 | Pyridine nitrogen is enriched with the preparation method of ultra-thin carbon nanosheet material and its metallic composite |
| CN110010366A (en) * | 2019-04-12 | 2019-07-12 | 东华大学 | A kind of nitrogen co-doped Nano carbon balls of fluorine-carbon nanosheet composite material and its preparation and application |
| RU197699U1 (en) * | 2019-07-03 | 2020-05-21 | Алексей Владимирович Сосунов | Hybrid carbon supercapacitor |
| CN114408903A (en) * | 2022-01-12 | 2022-04-29 | 华南理工大学 | Method for preparing in-plane porous few-layer graphene material at low temperature in environment-friendly manner |
| CN114560462A (en) * | 2022-02-28 | 2022-05-31 | 济南大学 | Preparation method of nitrogen and chlorine co-doped graphene |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110010366A (en) * | 2019-04-12 | 2019-07-12 | 东华大学 | A kind of nitrogen co-doped Nano carbon balls of fluorine-carbon nanosheet composite material and its preparation and application |
| RU197699U1 (en) * | 2019-07-03 | 2020-05-21 | Алексей Владимирович Сосунов | Hybrid carbon supercapacitor |
| CN114408903A (en) * | 2022-01-12 | 2022-04-29 | 华南理工大学 | Method for preparing in-plane porous few-layer graphene material at low temperature in environment-friendly manner |
| CN114560462A (en) * | 2022-02-28 | 2022-05-31 | 济南大学 | Preparation method of nitrogen and chlorine co-doped graphene |
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