CN110436457A - A kind of preparation method of supercapacitor N doping porous carbon electrode material - Google Patents
A kind of preparation method of supercapacitor N doping porous carbon electrode material Download PDFInfo
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- CN110436457A CN110436457A CN201910705334.1A CN201910705334A CN110436457A CN 110436457 A CN110436457 A CN 110436457A CN 201910705334 A CN201910705334 A CN 201910705334A CN 110436457 A CN110436457 A CN 110436457A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
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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
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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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
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
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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
- H01G11/44—Raw materials therefor, e.g. resins or coal
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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
The present invention relates to a kind of preparation methods of nitrogen-doped porous carbon material, the method for especially preparing nitrogen-doped porous carbon material as carbon source and nitrogen source using casein, further relate to its application and chemical property in super capacitor.Preparation method raw material sources convenience, is a kind of new way that nitrogen-doped porous carbon material is prepared using biomass at environmental protection, preparation step is simple, reaction condition is relatively mild, easily operated control, and large specific surface area, the specific capacitance for the N doping porous carbon prepared are high.The electrode material for super capacitor specific surface area prepared under the conditions of more excellent is up to 1902.5m2g‑1, nitrogen content is up to 8.3%, in 6M KOH solution, 1Ag‑1Under current density, specific capacitance is measured up to 393.2Fg‑1, and good cycling stability, it is a kind of electrode material for super capacitor of relative ideal.
Description
Technical field
The present invention relates to a kind of preparation methods of nitrogen-doped porous carbon material, especially prepare nitrogen as raw material using casein and mix
The method of miscellaneous porous carbon materials further relates to its application and chemical property in super capacitor.
Background technique
Currently, people increasingly compel the demand of renewable energy due to the pollution of environment and the consumption of fossil energy
It cuts, the development and utilization of renewable energy is of great significance to the energy crisis and environmental problem that solve current mankind society,
Solar energy, wind energy, water power that people develop now etc. are exactly a kind of environmentally friendly renewable energy.However, this kind of energy
With characteristics such as seasonal, regional and discontinuities, so that they cannot directly be used in industry and daily life.Cause
How this goes to store this kind of energy, becomes the hot issue nowadays studied.Common energy storage device has alkali currently on the market
The one-shot batteries such as manganese, silver-colored zinc, the secondary cells such as plumbic acid, ni-Cd, ni-mh and lithium ion battery are all whenever and wherever possible for a long time
The energy that convenient can be used, facilitates the production and living of people.However in the application scenarios such as some high energy pulses, this tradition
Battery be no longer satisfied required maximum power, it is therefore necessary to develop the energy storage device of high power density, come gram
Take this disadvantage of traditional energy storage device.Electrode material and electrolyte have vital effect in supercapacitor.Cause
For this two parts be measure a performance of the supercapacitor quality key component, decide supercapacitor energy density,
Power density and cyclical stability etc..In this two parts, electrode material is the hot issue of current researcher's research.It can use
Making super capacitor material mainly has this following several major class: carbon material (such as porous carbon, graphene, carbon nanotube)；Metal oxygen
Compound (such as RuO2, MnO2, CoOx, NiO, Fe2O3Deng)；Conducting polymer (polyaniline, polythiophene, polypyrrole etc.).And it is porous
Carbon is due to having the characteristics such as inexpensive, from a wealth of sources, no pollution to the environment, the big, excellent electrochemical performance of specific surface area aspect, In
There is greater advantage, thus the favor by numerous researchers in double layer capacitor.But the energy density of porous charcoal is low, to mention
The specific capacitance and energy density of high porous charcoal, the method generally used are to increase the specific surface area of porous charcoal, but specific surface area
Increase the decline that will lead to material conductivity, increases the internal resistance of supercapacitor；And use and introduce nitrogen into porous charcoal, it can
Increase the wetability between porous carbon material surface and electrolyte, fake capacitance reaction is introduced, to improve the specific capacitance of porous charcoal
[Chen Chong etc. prepares N doping porous charcoal based on sodium carboxymethylcellulose and its capacitive property is studied, Acta PhySico-Chimica Sinica, and 2013,
29 (1), 102-110], the document uses sodium carboxymethylcellulose for carbon source, and mixing urea outside is nitrogen source, through high temperature carbonization technique
N doping porous carbon material is prepared, the electrochemical capacitance performance of porous carbon material has obtained certain promotion, mass ratio electricity after N doping
Hold and 156.7F/g is increased to by 94.0F/g, but specific capacitance value or lower；For this purpose, it is proposed that one kind is with natural polymer-
Casein is the supplier of carbon source and nitrogen source, and nano silica is used to prepare electrode of super capacitor N doping carbon materials for template
The method of material, large specific surface area, the specific capacitance for the N doping porous carbon prepared are high.
Summary of the invention:
The present invention relates to a kind of preparation methods of nitrogen-doped carbon, especially prepare nitrogen-doped carbon material by raw material of casein
Method, the preparation method is simple, and easily operated control, low in cost, the specific surface area for the N doping porous carbon prepared
Greatly, specific capacitance is high.
One kind providing carbon source and nitrogen source prepares electrode of super capacitor nitrogen-doped carbon material using casein as raw material
Method, it is characterised in that carry out according to the following steps:
1. first dispersing quantitative casein in quantitative distilled water, it is added in quantitative silica solution, is stirred at 60 DEG C
30-60min is mixed to whole dissolutions, room temperature is cooled to, is transferred on polyfluortetraethylene plate, forced air drying 24 hours at 50 DEG C,
Casein/silica mixture is obtained, sample grind into powder is stand-by；Wherein casein performance indicator used are as follows: color
For white or milky；Fineness is in 30-200 mesh；Moisture is less than 12%；Ash content is less than 2.0%；PH value 4.0-4.6；Nitrogen pool
(N) 14-16%；The performance indicator of silica solution used are as follows: partial size 4-20nm；Content 15%；PH=12；Casein and silica solution are molten
Liquid usage ratio are as follows: mCasein∶mSilica solution=1: 2-6 (mass ratio) is 1: 3 (mass ratio) compared with ratio of greater inequality example；Casein and distilled water are used
Amount ratio are as follows: mCasein∶mDistilled water=1: 10-30 (mass ratio) is 1: 20 (mass ratio) compared with ratio of greater inequality example；
2. casein/silica mixture sample is placed in quartz boat and is put into tube type resistance furnace, in nitrogen protection
Under be carbonized, heating rate is 3-10 DEG C/min, is warming up to 600~900 DEG C, is carbonized 1~3 hour, then in nitrogen protection
Lower furnace cooling, is cooled to room temperature to it, and obtained product is placed in the NaOH solution of quantitative 3mol/L, soaks at 80 DEG C
It steeps 2h, then is washed with distilled water to PH=7,80 DEG C of dry 12h obtain N doping porous carbon (labeled as NC)；Wherein more excellent liter
Warm rate is 5 DEG C/min, and more excellent carburizing temperature is 800 DEG C, and more excellent carbonization time is 2 hours；
3. obtained N doping porous carbon (NC) is uniformly mixed with activator, be placed in tube furnace nitrogen protection into
Row activation, heating rate are 3-10 DEG C/min, are warming up to 600-900 DEG C of heat preservation 1h.Then furnace cooling under nitrogen protection, to
It is cooled to room temperature, and obtained sample 6mol/L hydrochloric acid is neutralized, then be washed with distilled water to PH=7,80 DEG C of dry 12h,
Obtain N doping porous carbon (labeled as ANC)；Wherein the activator is potassium hydroxide, lithium hydroxide, sodium hydroxide, carbonic acid
The mass ratio of one or more of mixture in lithium, sodium carbonate and potassium carbonate, N doping porous carbon (NC) and activator is 1: 1
~5；Wherein preferably activator is potassium hydroxide, and N doping porous carbon (NC) is more high quality than being 1: 3 with potassium hydroxide,
More excellent heating rate is 5 DEG C/min, and more excellent activation temperature is 800 DEG C；
4. by the N doping porous carbon (NC or ANC) of preparation and conductive black, polytetrafluoroethylene (PTFE) (PTFE) lotion according to 85:
The ratio of 10: 5 (mass ratioes) mixes, and is applied on the foam nickel screen collector of 1 millimeters thick, 1 × 1cm of application area uses tabletting
Machine is suppressed 15-30 seconds under 10MPa pressure；The electrode suppressed is put into 80 DEG C of dry 12h in electric drying oven with forced convection again, is dropped
To room temperature, electrode is put into the KOH solution of 6mol/L and is impregnated 12 hours, carries out cyclic voltammetry curve (CV), constant current fills
It discharges (GCD) and electrochemical AC impedance (EIS) is tested.
Specific embodiment of the present invention is as follows:
Below with reference to specific implementation example, the present invention will be further described, not limiting of its scope.Simultaneously
Experimental method described in following embodiments is unless otherwise specified conventional method；The reagent and material, such as without special
Illustrate, commercially obtains.
Embodiment 1: first dispersing 5 grams of casein in 100 milliliters of distilled water, is added in 16.7 grams of silica solution, In
35min is stirred at 60 DEG C to whole dissolutions, is cooled to room temperature, is transferred on polyfluortetraethylene plate, forced air drying 24 at 50 DEG C
Hour, casein/silica mixture is obtained, sample grind into powder is placed under tube furnace, under nitrogen protection, is risen
Warm rate is 5 DEG C/min, is warming up at 800 DEG C and keeps the temperature 2h.Obtained product is placed in the NaOH solution of 4mol/L, and 80 DEG C
Lower immersion 2h is washed to neutrality, and 80 DEG C of dry 12h obtain N doping porous carbon (NC), and scanning electron microscope is as shown in Fig. 1, warp
The specific surface area that specific surface tester measures N doping porous carbon is 609.3m2g-1, surveyed through x-ray photoelectron spectroscopy (XPS)
Nitrogen content be 7.4%.By obtained N doping porous carbon (NC) and conductive black, binder PTFE emulsion according to 85: 10: 5
Ratio mixing, be applied on the nickel screen of 1cm × 3cm, application area 1cm2.After impregnating 12h in 6M KOH solution, carry out
Cyclic voltammetry curve (CV), constant current charge-discharge (GCD) and electrochemical AC impedance (EIS) test.Attached drawing 6 shows electric double layer
Capacitance behavior；GCD (attached drawing 5b) discharge curve shows that NC electrode has preferable electrification close to corresponding charging curve is symmetrical with
Learn invertibity；The specific capacitance surveyed under the current density of 1A/g is 165F/g (attached drawing 7)；It can be seen that from attached drawing 8 in charging or discharging current
Density is after recycling 10000 times under 1A/g, and capacity retention ratio is up to 93.4%.
Embodiment 2:
It first disperses 5 grams of casein in 100 milliliters of distilled water, is added in 16.7 grams of silica solution, is stirred at 60 DEG C
35min is cooled to room temperature, is transferred on polyfluortetraethylene plate, forced air drying 24 hours, obtain at 50 DEG C to whole dissolutions
Sample grind into powder is placed under tube furnace by casein/silica mixture, under nitrogen protection, heating rate 5
DEG C/min, it is warming up at 800 DEG C and keeps the temperature 2h.Obtained N doping porous carbon and KOH are mixed in the ratio of 1: 3 (mass ratio)
It is even, it is placed on nitrogen protection in tube furnace, heating rate is 5 DEG C/min, is warming up to 80 DEG C of heat preservation 1h.The sample salt that will be obtained
Acid elution obtains N doping porous carbon (ANC), scanning electron microscope is as shown in Fig. 2, through specific surface to neutrality, 80 DEG C of dry 12h
The specific surface area that tester measures N doping porous carbon is 1912.1m2g-1, nitrogen, which is measured, through x-ray photoelectron spectroscopy (XPS) contains
Amount is 8.1%.Obtained ANC and conductive black, binder PTFE emulsion are mixed according to 85: 10: 5 ratio, are applied to 1cm
On the nickel screen of × 3cm, application area 1cm2.12h is impregnated in 6M KOH solution, the ratio electricity surveyed under the current density of 1A/g
Hold is 389.3F/g (attached drawing 7).After recycling 10000 times under charging or discharging current density is 1A/g, capacity retention ratio is up to
95.8% (attached drawing 8)；All discharge curves show that ANC electrode has preferable electricity close to corresponding charging curve is symmetrical with
Chemical invertibity (attached drawing 3)；Show as electric double layer capacitance behavior (attached drawing 4 and attached drawing 6)；Specific capacity with higher and fabulous
Cyclical stability.
Embodiment 3:
It first disperses 5 grams of casein in 120 milliliters of distilled water, is added in 22 grams of silica solution, is stirred at 60 DEG C
35min is cooled to room temperature, is transferred on polyfluortetraethylene plate, forced air drying 24 hours, are done at 50 DEG C to whole dissolutions
Sample grind into powder is placed under tube furnace by casein/silica mixture, under nitrogen protection, heating rate 5
DEG C/min, it is warming up at 800 DEG C and keeps the temperature 2h.Obtained N doping porous carbon and potassium carbonate is mixed in the ratio of 1: 4 (mass ratio)
It closes uniformly, is placed on nitrogen protection in tube furnace, heating rate is 5 DEG C/min, is warming up to 80 DEG C of heat preservation 1h.The sample that will be obtained
With salt acid elution to neutrality, 80 DEG C of dry 12h obtain N doping porous carbon (ANC3), measure N doping through specific surface tester
The specific surface area of porous carbon is 1897.4m2G, measuring nitrogen content through x-ray photoelectron spectroscopy (XPS) is 7.9%.It will obtain
ANC3 and conductive black, binder PTFE emulsion according to 85: 10: 5 ratio mix, be applied on the nickel screen of 1cm × 3cm,
Application area is 1cm2, 12h is impregnated in 6MKOH solution, the specific capacitance surveyed under the current density of 1A/g is 379.8F/g.
Embodiment 4:
It first disperses 5 grams of casein in 80 milliliters of distilled water, is added in 15 grams of silica solution, is stirred at 60 DEG C
45min is cooled to room temperature, is transferred on polyfluortetraethylene plate, forced air drying 24 hours, obtain at 50 DEG C to whole dissolutions
Sample grind into powder is placed under tube furnace by casein/silica mixture, under nitrogen protection, heating rate 5
DEG C/min, it is warming up at 800 DEG C and keeps the temperature 2h.By obtained N doping porous carbon and sodium hydroxide in the ratio of 1: 3 (mass ratio)
It is uniformly mixed, is placed on nitrogen protection in tube furnace, heating rate is 5 DEG C/min, is warming up to 80 DEG C of heat preservation 1h.The sample that will be obtained
Product salt acid elution to neutrality, 80 DEG C of dry 12h, obtains N doping porous carbon (ANC4), mixes through specific surface tester measurement nitrogen
The specific surface area of miscellaneous porous carbon is 1902.5m2g-1, measuring nitrogen content through x-ray photoelectron spectroscopy (XPS) is 8.3%.Will
The ANC4 and conductive black that arrive, binder PTFE emulsion are mixed according to 85: 10: 5 ratio, are applied to the nickel screen of 1cm × 3cm
On, application area 1cm2, 12h is impregnated in 6M KOH solution, the specific capacitance surveyed under the current density of 1A/g is
393.2F/g。
Detailed description of the invention:
Marginal data:
The stereoscan photograph of Fig. 1 .NC
The stereoscan photograph of Fig. 2 .ANC
Charging and discharging curve of Fig. 3 .ANC under different current densities
Cyclic voltammetry curve of Fig. 4 .ANC under different scanning rates
Charging and discharging curve of Fig. 5 .NC and ANC under 1A/g current density
Cyclic voltammetry curve of Fig. 6 .NC and ANC under 5mv/s sweep speed
Specific capacitance curve of Fig. 7 .NC from ANC under different current densities
Cyclical stability of Fig. 8 .NC and ANC under 1A/g current density.
Claims (7)
1. a kind of preparation method of supercapacitor nitrogen-doped porous carbon material is it is characterized in that, preparation method includes following step
It is rapid:
(1) it first disperses quantitative casein in quantitative distilled water, is added in quantitative silica solution, stirred at 60 DEG C
30-60min is cooled to room temperature, is transferred on polyfluortetraethylene plate, forced air drying 24 hours, obtain at 50 DEG C to whole dissolutions
To casein/silica mixture, sample grind into powder is placed in quartz boat and is put into tube type resistance furnace, protected in nitrogen
It is carbonized under shield, heating rate is 3-10 DEG C/min, is warming up to 600~800 DEG C, is carbonized 1~3 hour, is then protected in nitrogen
Lower furnace cooling is protected, is cooled to room temperature to it, obtained product is placed in the NaOH solution of 100 milliliters of 2-6mol/L, and 80
It impregnates 2h at DEG C, then is washed with distilled water to PH=7,80 DEG C of dry 12h obtain N doping porous carbon (labeled as NC)；
(2) obtained N doping porous carbon (NC) is uniformly mixed with activator, is placed in tube furnace and is carried out in nitrogen protection
Activation, heating rate are 3-10 DEG C/min, are warming up to 600-800 DEG C of heat preservation 1h.Then furnace cooling under nitrogen protection, to it
It is cooled to room temperature, obtained sample 6mol/L hydrochloric acid is neutralized, then be washed with distilled water to PH=7,80 DEG C of dry 12h are obtained
To N doping porous carbon (being labeled as ANC).
2. the preparation method described according to claim 1, it is characterised in that casein performance indicator are as follows: color be white or
Milky；Fineness is in 30-200 mesh；Moisture is less than 12%；Ash content is less than 2.0%；PH value 4.0-4.6；Nitrogen pool (N), %14.5
~15.5,15-16.
3. the preparation method described according to claim 1, it is characterised in that the performance indicator of silica solution are as follows: partial size 4-
20nm；Content 15%；PH=12.
4. the preparation method described according to claim 1, it is characterised in that casein and silicon sol solution usage ratio are as follows:
mCasein∶mSilica solution=1: 2-6 (mass ratio).
5. the preparation method described according to claim 1, it is characterised in that casein and distilled water usage ratio are as follows: mCasein
∶mDistilled water=1: 10-30 (mass ratio).
6. the preparation method described according to claim 1, it is characterised in that the activator is potassium hydroxide, hydroxide
One or more of mixture in lithium, sodium hydroxide, lithium carbonate, sodium carbonate and potassium carbonate；The N doping porous carbon (NC)
Mass ratio with activator is 1: 1~5.
7. the N doping porous carbon prepared according to claim 1 and conductive black, polytetrafluoroethylene (PTFE) (PTFE) lotion are according to 85: 10
: the ratio mixing of 5 (mass ratioes) is applied on the foam nickel screen collector of 1 millimeters thick, 1 × 1cm of application area uses tablet press machine
It is suppressed 30 seconds under 10MPa pressure, then is put into 80 DEG C of dry 12h in electric drying oven with forced convection, be down to room temperature, super capacitor is made
Device electrode material.
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