CN109205620A - A kind of carbon bionic nano material and preparation method - Google Patents
A kind of carbon bionic nano material and preparation method Download PDFInfo
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- CN109205620A CN109205620A CN201811363705.4A CN201811363705A CN109205620A CN 109205620 A CN109205620 A CN 109205620A CN 201811363705 A CN201811363705 A CN 201811363705A CN 109205620 A CN109205620 A CN 109205620A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 42
- 239000011664 nicotinic acid Substances 0.000 title claims abstract description 26
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 54
- 241000219138 Luffa Species 0.000 claims abstract description 17
- 235000003956 Luffa Nutrition 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 15
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000012190 activator Substances 0.000 claims abstract description 14
- 230000004913 activation Effects 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- 229910003481 amorphous carbon Inorganic materials 0.000 claims abstract description 4
- 239000013078 crystal Substances 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000003763 carbonization Methods 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000010453 quartz Substances 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 7
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000002604 ultrasonography Methods 0.000 claims description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 5
- 229910052700 potassium Inorganic materials 0.000 claims description 5
- 239000011591 potassium Substances 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 20
- 239000000126 substance Substances 0.000 abstract description 15
- 239000002994 raw material Substances 0.000 abstract description 7
- 230000003213 activating effect Effects 0.000 abstract description 4
- 230000005540 biological transmission Effects 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 abstract 1
- 244000302544 Luffa aegyptiaca Species 0.000 description 11
- 235000009814 Luffa aegyptiaca Nutrition 0.000 description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- 239000012299 nitrogen atmosphere Substances 0.000 description 8
- 239000002250 absorbent Substances 0.000 description 6
- 230000002745 absorbent Effects 0.000 description 6
- 239000003610 charcoal Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000005611 electricity Effects 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 5
- 238000010408 sweeping Methods 0.000 description 5
- 239000003575 carbonaceous material Substances 0.000 description 4
- 239000007772 electrode material Substances 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 239000006260 foam Substances 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 238000002484 cyclic voltammetry Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 239000002023 wood Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- HEFNNWSXXWATRW-UHFFFAOYSA-N Ibuprofen Chemical compound CC(C)CC1=CC=C(C(C)C(O)=O)C=C1 HEFNNWSXXWATRW-UHFFFAOYSA-N 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- 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
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of carbon bionic nano material and preparation methods.The carbon bionic nano material is using luffa as raw material, and using potassium hydroxide chemical activation method, the active carbon with high specific surface area material (AC) prepared under conditions of different temperature and different activating substance ratios, maximum specific surface area is 1592m2/ g is mainly made of the amorphous carbon of exposure { 002 } and { 100 } crystal face.Preparation method is to carry out cleaning and crush drying process first to luffa, the luffa after drying is carbonized with tube furnace, then it is activated under different temperatures and different activating substance ratios with activator potassium hydroxide, finally drying can be prepared by sample after persulfuric acid and deionized water processing.Carbon bionic nano material leaves a large amount of gaps after being activated on the surface of the material in the present invention, the specific surface area of material can be increased, improve transmission rate of the ion in charge and discharge process, can at higher current densities charge and discharge when keep higher capacitance.
Description
Technical field
The invention belongs to carbon bionic nano material electrode material technical field, it is related to a kind of carbon bionic nano material and preparation
Method more particularly to a kind of system for the carbon bionic nano material for easily being obtained with raw material and being easy preparation and large specific surface area
It is standby, it can be used for electrode material for super capacitor.
Background technique
Due to well-known, the energy based on fossil fuel causes many economy and environment in the world
Problem.Ever-increasing energy demand, the resource consumption of fossil fuel and more and more environmental problems, including greenhouse gas
The discharge of body discharge and region air pollutants, all promoting people to seek exploitation has replacing for high power density and energy density
For the energy.Meanwhile with the continuous development of technology, people are also constantly promoting the demand of high-performance energy storage device.At this
Under kind of historical background, there is supercapacitor, and many materials is made to be used for the research of electrode of super capacitor, and wherein
Carbon material is search time longest, widest material.In the industrial course of electrode carbon material, biomass raw material are present
It has been increasingly becoming active carbon, the primary raw material of porous carbon.
Active carbon has permanent industrial production and applicating history, is applied to the carbon electrode material of supercapacitor earliest,
And porous carbon-activity powdered carbon-activated carbon fibre this sequence, represent active carbon industrial expansion direction because material pass through
After overactivation, micropore quantity can be obviously improved, to improve the utilization rate of active carbon.Ellie Yi Lih Teo et al. is used
Activation of potassium hydroxide method prepares rice hull active carbon (RHAC), and specific surface area is up to 2696m2/ g, SEM and TEM figure prove its carbon
The mesoporous quantity of powder is obviously improved, and advantageously forms electric double layer；Essandoh et al. is had by high temperature pyrolysis matsuki article
The activated carbon of multi-cellular structure.The experimental results showed that matsuki article active carbon wants the salicylic acid in waste water with brufen adsorption capacity
Much higher than commercial activated carbons；Porous carbon has been made with hydro-thermal method under the conditions of 300 DEG C using discarded pine and rice husk in Liu et al. people
Material；For Shoaib and Al-SWaidan using date as raw material, carbon dioxide is activated gas, keeps the temperature 30min under high pressure, obtains
Specific surface area is 1094m2The porous carbon materials of/g.
Summary of the invention
The purpose of the invention is to increase the specific surface area of carbon bionic nano material, to improve its chemical property.
Thus for the first time using luffa as the raw material of carbon bionic nano material, and material is improved using potassium hydroxide chemical activation method
Specific surface area prepares the absorbent charcoal material with high-specific surface area.
Technical purpose of the invention is achieved by following technical proposals:
A kind of preparation method of carbon bionic nano material, includes the following steps:
(1) luffa is cut into small pieces, is cleaned with deionized water and ethyl alcohol, it is dry complete in thermostatic drying chamber；
(2) luffa in step (1) after drying is taken to be put into quartz boat, with not under inert gas shielding in tube furnace
Heating rate higher than 5 DEG C/min is heated to 400 DEG C and is carbonized, and keeps 4h；
(3) it takes the sample being carbonized in step (2) and activator potassium hydroxide is added, deionized water, which is added, makes its mixing, stirs
Mixing is uniformly mixed it, and mixed liquor is put into baking oven later, is completely dried, and guarantees the sample and activator hydrogen of the carbonization being added
The mass ratio of potassium oxide is 1:1~4；
(4) sample after will be dry in step (3) is ground uniformly in mortar, is put into quartz boat, lazy in tube furnace
Property gas shield under, carry out activation 70min at 600~800 DEG C, heating rate is not higher than 5 DEG C/min, cooled to room temperature；
(5) 1M H is used2SO4Sample obtained by step (4) is cleaned twice, every time ultrasound at least 15min after mixing, so
It is washed with ethyl alcohol and deionized water to neutrality, is dried in vacuo at 60 DEG C afterwards, gained sample is carbon bionic nano material.
Further, the sample for the carbonization being added in step (3) and the mass ratio of activator potassium hydroxide are 1:2.
Further, it under inert gas shielding, is activated at 700 DEG C in tube furnace in step (4).
Further, mixing time is no less than 1h in step (3), so that sample and activator are uniformly mixed.
Further, in step (2) and (4), the inert gas is one kind of nitrogen or argon gas, so as in calcination process
Carbon bionic nano material it is not oxidized fall.
The above-mentioned carbon bionic nano material maximum specific surface area is 1576m2/ g, mainly by exposure { 002 } and { 100 } crystal face
Amorphous carbon composition.
The luffa that do not studied present invention employs forefathers prepares carbon nanotube biomimic material as raw material, and sponge gourd is
One of the crops that China is planted extensively, the luffa fibers after luffa, that is, sponge gourd maturation aging.Luffa itself have compared with
Big specific surface area, fibre structure abundant, and the experimental results showed that counterfeit electricity can be served as containing more nickel element in sponge gourd
Hold, theoretically good electrode material.Luffa environmental protection, it is economical, it easily obtains, yield is larger, there is the potentiality of industrial applicability.This
Invention uses potassium hydroxide chemical activation method, and the ratio of material is improved under different activation temperatures and different activating substance ratios
Surface area prepares the absorbent charcoal material with high-specific surface area, to have excellent chemical property.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of 2 product of the embodiment of the present invention；(a) 5 μ m in size, (b) 500nm size.
Fig. 2 is 2 product examination of infrared spectrum figure of the embodiment of the present invention；
Fig. 3 is 2 product specific surface area test chart of the embodiment of the present invention；(a) adsorption/desorption curve, (b) pore-size distribution.
Fig. 4 is the X-ray diffractogram of 2 product of the embodiment of the present invention；
Fig. 5 is the chemical property figure of 2 product of the embodiment of the present invention；(a) different temperatures, (b) different scanning speed, (c)
Different current densities, (b) loop test.
Specific embodiment
Below by specific example and attached drawing, the present invention will be further elaborated, it should explanation, following the description
It is intended merely to explain the present invention, its content not limited.
Embodiment 1
It takes the luffa bought to clean, is cut into fritter appropriate, dried for 24 hours at 100 DEG C.Sponge gourd after drying takes 10g
It is put into quartz boat, is heated to 400 DEG C under nitrogen atmosphere in tube furnace with the heating rate of 5 DEG C/min and is carbonized, keep
4h, the sample after carbonization are denoted as sponge gourd carbon (SC).Activator potassium hydroxide is added in the sample of carbonization, so that the hydrogen-oxygen being added
The mass ratio of sample after changing potassium and carbonization is 1:1, and deionized water, which is added, makes its mixing, and stirring 1h is uniformly mixed it, later
Mixed liquor is put into baking oven, is dried for 24 hours at 100 DEG C.Sample grinding after drying is uniformly put into quartz boat, in tubular type
In furnace under nitrogen atmosphere, 70min, 5 DEG C/min of heating rate, cooled to room temperature are activated at 700 DEG C.Sample after activation
With 1M H2SO4Ultrasound 15min after mixing twice and every time is washed, is then rinsed with deionized water and ethyl alcohol to neutrality, at 60 DEG C very
Sky is dry, collects sample.It takes absorbent charcoal material prepared by 8mg, 1mg conductive black, 1mgPVDF to be uniformly mixed in mortar to apply
Onto processed nickel foam, electrode is made in tabletting after being dried in vacuo at 60 DEG C, makees electrolyte, Hg/HgO electricity with 6M KOH
Extremely reference electrode, Pt electrode are the chemical property that comparison electrode surveys made electrode.Through cyclic voltammetry, with the composite wood
Expect that the electrode prepared maximum capacitance when sweeping speed and being 5mV/s is 170F/g.
Embodiment 2
It takes the luffa bought to clean, is cut into fritter appropriate, dried for 24 hours at 100 DEG C.Sponge gourd after drying takes 10g
It is put into quartz boat, is heated to 400 DEG C under nitrogen atmosphere in tube furnace with the heating rate of 5 DEG C/min and is carbonized, keep
4h, the sample after carbonization are denoted as sponge gourd carbon (SC).Activator potassium hydroxide is added in the sample of carbonization, so that the hydrogen-oxygen being added
The mass ratio of sample after changing potassium and carbonization is 2:1, and deionized water, which is added, makes its mixing, and stirring 1h is uniformly mixed it, later
Mixed liquor is put into baking oven, is dried for 24 hours at 100 DEG C.Sample grinding after drying is uniformly put into quartz boat, in tubular type
In furnace under nitrogen atmosphere, 70min, 5 DEG C/min of heating rate, cooled to room temperature are activated at 700 DEG C.Sample after activation
With 1M H2SO4Ultrasound 15min after mixing twice and every time is washed, is then rinsed with deionized water and ethyl alcohol to neutrality, at 60 DEG C very
Sky is dry, collects sample.It takes absorbent charcoal material prepared by 8mg, 1mg conductive black, 1mgPVDF to be uniformly mixed in mortar to apply
Onto processed nickel foam, electrode is made in tabletting after being dried in vacuo at 60 DEG C, makees electrolyte, Hg/HgO electricity with 6M KOH
Extremely reference electrode, Pt electrode are the chemical property that comparison electrode surveys made electrode.Attached drawing 1 is the present embodiment products therefrom
Scanning electron microscope (SEM) photograph, as seen from the figure, the carbon bionic nano material prepared are bulk, in blocky surface cloth after activation of potassium hydroxide
Aperture is expired, to increase the specific surface area of material；Attached drawing 2 is the examination of infrared spectrum figure of the present embodiment products therefrom, by scheming
It is found that there are several functional groups, mainly C=C aromatic gp in the sample；Attached drawing 3 is the specific surface of the present embodiment products therefrom
Product test chart, the specific surface area of the product known to Fig. 3 a are 1592m2/ g, Fig. 3 b are the carbon bionic nano material surface aperture
Graph of pore diameter distribution, it is known that aperture is 4nm or so；Attached drawing 4 is the X-ray diffractogram of the present embodiment products therefrom, as seen from the figure,
The material is mainly made of the amorphous carbon of exposure { 002 } and { 100 } crystal face；Attached drawing 5 is the electrification of the present embodiment products therefrom
Performance map is learned, Fig. 5 a is the cyclic voltammetric of the carbon nanotube biomimic material that activates at different temperatures when sweeping speed and being 50mV/s
Figure, its chemical property is best when activating at 700 DEG C as seen from the figure；Fig. 5 b is the carbon bionic nano activated at 700 DEG C
The test of material circulation volt-ampere, when sweeping speed and being 5mV/s, maximum capacitance is 222F/g, illustrates that it is forthright with good times
Can, Fig. 5 c is its charge-discharge test, and in current density 1A/g, specific capacitance is 236F/g；Fig. 5 d is charge and discharge under constant current density
Electric loop test is up to 95% by the circle circulation capacitance retention rate of charge and discharge 10000 at current density 10A/g.Experiment knot
Fruit proves that the bionical carbon material of this method preparation has excellent chemical property.
Embodiment 3
It takes the luffa bought to clean, is cut into fritter appropriate, dried for 24 hours at 100 DEG C.Sponge gourd after drying takes 10g
It is put into quartz boat, is heated to 400 DEG C under nitrogen atmosphere in tube furnace with the heating rate of 5 DEG C/min and is carbonized, keep
4h, the sample after carbonization are denoted as sponge gourd carbon (SC).Activator potassium hydroxide is added in the sample of carbonization, so that the hydrogen-oxygen being added
The mass ratio of sample after changing potassium and carbonization is 3:1, and deionized water, which is added, makes its mixing, and stirring 1h is uniformly mixed it, later
Mixed liquor is put into baking oven, is dried for 24 hours at 100 DEG C.Sample grinding after drying is uniformly put into quartz boat, in tubular type
In furnace under nitrogen atmosphere, 70min, 5 DEG C/min of heating rate, cooled to room temperature are activated at 700 DEG C.Sample after activation
With 1M H2SO4Ultrasound 15min after mixing twice and every time is washed, is then rinsed with deionized water and ethyl alcohol to neutrality, at 60 DEG C very
Sky is dry, collects sample.It takes absorbent charcoal material prepared by 8mg, 1mg conductive black, 1mgPVDF to be uniformly mixed in mortar to apply
Onto processed nickel foam, electrode is made in tabletting after being dried in vacuo at 60 DEG C, makees electrolyte, Hg/HgO electricity with 6M KOH
Extremely reference electrode, Pt electrode are the chemical property that comparison electrode surveys made electrode.Through cyclic voltammetry, with the composite wood
Expect that the electrode prepared maximum capacitance when sweeping speed and being 5mV/s is 167F/g.
Embodiment 4
It takes the luffa bought to clean, is cut into fritter appropriate, dried for 24 hours at 100 DEG C.Sponge gourd after drying takes 10g
It is put into quartz boat, is heated to 400 DEG C under nitrogen atmosphere in tube furnace with the heating rate of 5 DEG C/min and is carbonized, keep
4h, the sample after carbonization are denoted as sponge gourd carbon (SC).Activator potassium hydroxide is added in the sample of carbonization, so that the hydrogen-oxygen being added
The mass ratio of sample after changing potassium and carbonization is 4:1, and deionized water, which is added, makes its mixing, and stirring 1h is uniformly mixed it, later
Mixed liquor is put into baking oven, is dried for 24 hours at 100 DEG C.Sample grinding after drying is uniformly put into quartz boat, in tubular type
In furnace under nitrogen atmosphere, 70min, 5 DEG C/min of heating rate, cooled to room temperature are activated at 700 DEG C.Sample after activation
With 1M H2SO4Ultrasound 15min after mixing twice and every time is washed, is then rinsed with deionized water and ethyl alcohol to neutrality, at 60 DEG C very
Sky is dry, collects sample.It takes absorbent charcoal material prepared by 8mg, 1mg conductive black, 1mgPVDF to be uniformly mixed in mortar to apply
Onto processed nickel foam, electrode is made in tabletting after being dried in vacuo at 60 DEG C, makees electrolyte, Hg/HgO electricity with 6M KOH
Extremely reference electrode, Pt electrode are the chemical property that comparison electrode surveys made electrode.Through cyclic voltammetry, with the composite wood
Expect that the electrode prepared maximum capacitance when sweeping speed and being 5mV/s is 179F/g.
Claims (9)
1. a kind of preparation method of carbon bionic nano material, which comprises the steps of:
(1) luffa is cut into small pieces, is cleaned with deionized water and ethyl alcohol, it is dry complete in thermostatic drying chamber；
(2) luffa in step (1) after drying is taken to be put into quartz boat, to be not higher than under inert gas shielding in tube furnace
The heating rate of 5 DEG C/min is heated to 400 DEG C and is carbonized, and keeps 4h；
(3) it takes the sample being carbonized in step (2) and activator potassium hydroxide is added, deionized water, which is added, makes its mixing, and stirring makes
It is uniformly mixed, and mixed liquor is put into baking oven later, is completely dried, and guarantees the sample and activator hydroxide of the carbonization being added
The mass ratio of potassium is 1:1~4；
(4) sample after will be dry in step (3) is ground uniformly in mortar, is put into quartz boat, the indifferent gas in tube furnace
Under body protection, activation 70min is carried out at 600~800 DEG C, heating rate is not higher than 5 DEG C/min, cooled to room temperature；
(5) 1M H is used2SO4Sample obtained by step (4) is cleaned twice, ultrasound at least 15min after mixing, is then used every time
Ethyl alcohol and deionized water are washed to neutrality, are dried in vacuo at 60 DEG C, and gained sample is carbon bionic nano material.
2. the preparation method of carbon bionic nano material according to claim 1, which is characterized in that be added in step (3)
The sample of carbonization and the mass ratio of activator potassium hydroxide are 1:2.
3. the preparation method of carbon bionic nano material according to claim 1 or 2, which is characterized in that in pipe in step (4)
In formula furnace under inert gas shielding, activated at 700 DEG C.
4. preparation method according to claim 1 or 2, which is characterized in that mixing time cannot be less than 1h in step (3),
So that sample and activator are uniformly mixed.
5. preparation method according to claim 3, which is characterized in that mixing time is no less than 1h in step (3), so as to sample
Product and activator are uniformly mixed.
6. preparation method described according to claim 1 or 2 or 5, which is characterized in that in step (2) and (4), the indifferent gas
Body is one kind of nitrogen or argon gas, so as to calcination process carbon bionic nano material it is not oxidized fall.
7. preparation method according to claim 3, which is characterized in that in step (2) and (4), the inert gas is nitrogen
One kind of gas or argon gas, so as to calcination process carbon bionic nano material it is not oxidized fall.
8. the preparation method according to claim 4, which is characterized in that in step (2) and (4), the inert gas is nitrogen
One kind of gas or argon gas, so as to calcination process carbon bionic nano material it is not oxidized fall.
9. carbon bionic nano material made from claim 1-8 either method, which is characterized in that the carbon bionic nano material is maximum
Specific surface area is 1592m2/ g is mainly made of the amorphous carbon of exposure { 002 } and { 100 } crystal face.
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| CN112670097A (en) * | 2021-01-05 | 2021-04-16 | 齐鲁工业大学 | Preparation method of loofah sponge-based derived carbon electrode material with three-dimensional network structure |
| CN112811892A (en) * | 2021-03-01 | 2021-05-18 | 山东大学 | Preparation method of silk melon flesh-like collateral bone scaffold |
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| CN113880083A (en) * | 2021-10-27 | 2022-01-04 | 中冶集团武汉勘察研究院有限公司 | Method for preparing biomass activated carbon by utilizing loofah sponge |
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