CN107055530A - Pumpkin derives stratiform carbon as the preparation method of electrode material for super capacitor - Google Patents
Pumpkin derives stratiform carbon as the preparation method of electrode material for super capacitor Download PDFInfo
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- CN107055530A CN107055530A CN201710311848.XA CN201710311848A CN107055530A CN 107055530 A CN107055530 A CN 107055530A CN 201710311848 A CN201710311848 A CN 201710311848A CN 107055530 A CN107055530 A CN 107055530A
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- pumpkin
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- carbonized
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- carbon material
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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
-
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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 pumpkin derives stratiform carbon as the preparation method of electrode material for super capacitor, it is characterised in that comprise the following steps：1) feeding：Fresh pumpkin is removed into surface and seed, the pumpkin of yellow is obtained, the thin slice that thickness is 0.1 3mm is whittled into；2) dry：Above-mentioned thin slice is freeze-dried 12 24 hours at 0~50 DEG C；3) it is carbonized：Thin slice after freeze-drying process is carbonized at 600 1000 DEG C, soaking time 1 10 hours leads to inert gas shielding；4) activate：Carbonized product is put into 2 7M KOH solution and soaked 13 days, the mass ratio of KOH solution and carbonized product is 5:1 to 1:1；The carbon of immersion is taken out drying, tube furnace activation is put into, activation condition is：Calcined 15 hours at 600 1000 DEG C, and logical inert gas shielding, room temperature is finally dropped to, the sylvite of residual is cleaned with 0.1M HCl, the pumpkin for obtaining layered porous structure derives stratiform carbon material；Above method raw material it is cheap and easy to get, easy to operation and prepare pumpkin derive carbon material there is layer structure, specific surface area is big.
Description
Technical field
The present invention relates to electrode material for super capacitor technical field, more particularly to pumpkin derivative stratiform carbon is used as super electricity
The preparation method of container electrode material.
Background technology
Ultracapacitor have power density it is high (>10kW/kg), service life length (>105 times) and the discharge and recharge time it is short
The advantage of (tens seconds), has been widely used for the fields such as electronic equipment and hybrid electric vehicle, with the swift and violent hair of clean energy resource
Exhibition and the continuous improvement of automotive performance, performance and cost requirement more and more higher for electrode material for super capacitor.Current business
Electrode material for super capacitor is manganese oxide system mostly, although the theoretical capacity of manganese oxide electrode is high, but it is followed
Ring stability is poor, by the discharge and recharge of thousands of times, and its capacity attenuation is serious, and service life is shorter.And carbon-based electrode material
Service life is very long, is used by the charge and discharge cycles of tens of thousands of times, capacity, which remains unchanged, is maintained at more than 90%；And carbon material is led
Electrically good, as electrode material, it has good high rate performance；Carbon material chemical stability is good, energy acid-fast alkali-proof, and nothing
Poison, therefore with huge electrode for capacitors application prospect.Current major part activated carbon is as the specific capacity of capacitor in 200F/
G, with the development of the high Energy device such as electric car, the energy density to capacitor requires also more and more higher, it is therefore desirable to improve
Its specific capacity.
Pumpkin abundance, its composition is mainly carbon, hydrogen and oxygen, and it has as the latent of biomass derived carbon material
Power.
The content of the invention
It is an object of the invention to rationally derive stratiform carbon material there is provided a kind of pumpkin by the use of pumpkin resource to be used as super electricity
The preparation method of container electrode material.
A kind of pumpkin derives stratiform carbon as the preparation method of electrode material for super capacitor, comprises the following steps：
1) feeding：Fresh pumpkin is removed into surface and seed, the pumpkin of yellow is obtained, it is 0.1-3mm's to be whittled into thickness
Thin slice；
2) dry：Above-mentioned thin slice is freeze-dried 12-24 hours at 0~-50 DEG C；
3) it is carbonized：Thin slice after freeze-drying process is carbonized at 600-1000 DEG C, soaking time 1-10 hours is led to lazy
Property gas shield；
4) activate：Carbonized product is put into 2-7M KOH solution and soaked 1-3 days, the mass ratio of KOH and carbonized product is
5:1 to 1:1；The carbon of immersion is taken out drying, tube furnace activation is put into, activation condition is：1-5 is calcined at 600-1000 DEG C small
When, and logical inert gas shielding, room temperature is finally dropped to, the sylvite of residual is cleaned with 0.1M HCl, layered porous structure is obtained
Pumpkin derives stratiform carbon material.
Preferably, the inert gas is argon gas or nitrogen.
Preferably, the heating rate of the high-temperature calcination is 1-15 DEG C/min.
Preferably, the inert atmosphere is Ar or N2Atmosphere.
Preferably, described layer structure pumpkin derives carbon material, and its specific surface area is more than 2000m2/ g, as super electricity
Container electrode material constant current discharge specific capacity under 1A/g is more than 5000 capacity of constant current charge-discharge under 300F/g, 10A/g
It is undamped.
The advantage of the invention is that：
1) raw material is cheap and easy to get；
2) it is easy to operation；
3) pumpkin prepared, which derives carbon material, has layer structure, and specific surface area is big；
4) when the layered porous pumpkin derives carbon material as electrode material for super capacitor, with specific capacity height, multiplying power
The advantage of performance and good cycling stability.
Brief description of the drawings
Fig. 1 is that pumpkin of the present invention derives stratiform carbon as the preferred embodiment of preparation method one of electrode material for super capacitor
Flow chart.
Fig. 2 is the XRD of the derivative carbon material prepared in embodiments of the invention 1 to 4.
Fig. 3 is the SEM figures of the derivative carbon material prepared in embodiments of the invention 1 to 4.
Fig. 4 is the constant current charge-discharge curve map of the derivative carbon material prepared in embodiments of the invention 1 to 4.
Fig. 5 is the cyclic voltammetry curve of the derivative carbon material prepared in embodiments of the invention 1 to 4.
Fig. 6 is the constant current cycle charge discharge electrograph of the derivative carbon material prepared in embodiments of the invention 1 to 4.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with accompanying drawing to embodiment party of the present invention
Formula is further described.
The present invention is described in further detail with reference to embodiment and accompanying drawing.
Embodiment 1：
1) feeding：Fresh pumpkin is removed into surface and seed, the pumpkin of yellow is obtained, it is the thin of 0.1cm to be whittled into thickness
Piece.
2) dry：Above-mentioned thin slice is freeze-dried 24 hours at 0 DEG C.
3) it is carbonized：Thin slice after freeze-drying process is carbonized at 600 DEG C and obtains carbide, by carbide soaking time
2 hours, lead to nitrogen protection.
4) activate：Carbonized product is put into 2M (mole every liter) KOH (potassium hydroxide) solution and soaked 3 days, KOH solution with
The mass ratio of carbonized product is 5：1；The carbonized product of immersion is taken out drying, tube furnace activation is put into, activation condition is：700
Calcined 5 hours at DEG C, and logical nitrogen protection, room temperature is finally dropped to, the sylvite of residual is cleaned with 0.1M HCl (hydrogen chloride solution),
The pumpkin for obtaining layered porous structure derives stratiform carbon material.
5) electrochemical property test：Pumpkin obtained above is tested using aqueous phase three-electrode system and derives stratiform carbon material
Chemical property, wherein prepared pumpkin, which derives stratiform carbon material, makes working electrode, it is ginseng to electrode, Hg/HgO that platinized platinum, which is,
Than electrode, electrolyte is 6M KOH solution, and tester is Shanghai morning CHI 760E electrochemical workstations；Test result is such as
Shown in accompanying drawing 4-6.
Embodiment 2：
1) feeding:Fresh pumpkin is removed into surface and seed, the pumpkin of yellow is obtained, it is the thin of 0.5mm to be whittled into thickness
Piece.
2) dry：Above-mentioned thin slice is freeze-dried 20 hours at -10 DEG C.
3) it is carbonized：Thin slice after freeze-drying process is carbonized at 700 DEG C, soaking time 8 hours is led to argon gas and protected
Shield.
4) activate：Carbonized product is put into 3M KOH solutions and soaked 3 days, the mass ratio of KOH solution and carbonized product is
4：1；The carbonized product of immersion is taken out drying, tube furnace activation is put into, activation condition is：Calcine 4 hours, and lead at 700 DEG C
Argon gas is protected, and finally drops to room temperature, and the sylvite of residual is cleaned with 0.1M HCl, and the pumpkin for obtaining layered porous structure derives stratiform
Carbon material.
5) electrochemical property test：Its method of testing be the same as Example 1.
Embodiment 3：
1) feeding：Fresh pumpkin is removed into surface and seed, the pumpkin of yellow is obtained, the thin slice that thickness is 1mm is whittled into.
2) dry：Above-mentioned thin slice is freeze-dried 15 hours at -20 DEG C.
3) it is carbonized：Thin slice after freeze-drying process is carbonized at 9000 DEG C, soaking time 5 hours leads to nitrogen protection.
4) activate：Carbonized product is put into 5M KOH solutions and soaked 2 days, the mass ratio of KOH solution and carbonized product is
3:1；The carbonized product of immersion is taken out drying, tube furnace activation is put into, activation condition is：Calcine 2 hours, and lead at 900 DEG C
Nitrogen is protected, and finally drops to room temperature, and the sylvite of residual is cleaned with 0.1M HCl, and the pumpkin for obtaining layered porous structure derives stratiform
Carbon material.
5) electrochemical property test：Its method of testing be the same as Example 1.
Embodiment 4：
1) feeding:Fresh pumpkin is removed into surface and seed, the pumpkin of yellow is obtained, the thin slice that thickness is 3mm is whittled into.
2) dry：Above-mentioned thin slice is freeze-dried 12 hours at -50 DEG C.
3) it is carbonized：Thin slice after freeze-drying process is carbonized at 1000 DEG C, soaking time 1 hour leads to argon gas protection.
4) activate：Carbonized product is put into 7M KOH solutions and soaked 1 day, the mass ratio of KOH and carbonized product is 1：1；
The carbonized product of immersion is taken out drying, tube furnace activation is put into, activation condition is：Calcined 1 hour at 1000 DEG C, and logical argon gas
Protection, finally drops to room temperature, and the sylvite of residual is cleaned with 0.1M HCl, and the pumpkin for obtaining layered porous structure derives stratiform carbon materials
Material.
5) electrochemical property test：Its method of testing be the same as Example 1.
Referring to accompanying drawing, Fig. 2 is the XRD of the pumpkin derivative carbon material prepared in embodiment 1 to 4.Wherein, abscissa is angle
Degree；Ordinate is relative intensity.It can be seen from the figure that is to have weaker graphite diffraction maximum at 25 ° in 2 θ, so as to prove what is obtained
Product is amorphous carbon material,.
Fig. 3 is the SEM figures of the pumpkin derivative carbon material prepared in embodiment 1 to 4.This carbon material as we can see from the figure
For layer structure, and layer very thin thickness；Therefore it has great specific surface area, and this is conducive to the diffusion contact of ion, can be with
Improve the capacity of ultracapacitor.
Fig. 4 is the constant current charge-discharge curve map of the pumpkin derivative carbon material prepared in embodiment 1 to 4.Can be with from figure
Find out, under 1A/g current density, the discharge and recharge time is basic in 380s or so, and specific capacity is up to 380F/g.
Fig. 5 is the cyclic voltammetry curve of the pumpkin derivative carbon material prepared in embodiment 1 to 4.It can be seen that
20mV s-1Sweep under speed, it remains unchanged holding rectangular curve, illustrates that it has preferable electric double layer energy storage characteristic.
Fig. 6 is the stable circulation linearity curve of the pumpkin derivative carbon material prepared in embodiment 1 to 4.It is close in 10A/g electric current
Under degree, after 5000 times circulate, the conservation rate of specific capacity is up to 99%, illustrates that it has good cyclical stability.
The present invention does not limit to above-mentioned cited embodiment, and those skilled in the art can be according to the present invention
Operation principle and embodiment given above, can make it is various it is equivalent change, equivalent replacement, part increase and decrease and
Reconfigure, so as to constitute more new embodiments.
Claims (5)
1. a kind of pumpkin derives stratiform carbon as the preparation method of electrode material for super capacitor, it is characterised in that including as follows
Step：
1) feeding：Fresh pumpkin is removed into surface and seed, the pumpkin of yellow is obtained, the thin slice that thickness is 0.1-3mm is whittled into；
2) dry：Above-mentioned thin slice is freeze-dried 12-24 hours at 0~-50 DEG C；
3) it is carbonized：Thin slice after freeze-drying process is carbonized at 600-1000 DEG C, soaking time 1-10 hours leads to indifferent gas
Body is protected；
4) activate：Carbonized product is put into 2-7M KOH solution and soaked 1-3 days, the mass ratio of KOH solution and carbonized product is
5:1 to 1:1；The carbon of immersion is taken out drying, tube furnace activation is put into, activation condition is：1-5 is calcined at 600-1000 DEG C small
When, and logical inert gas shielding, room temperature is finally dropped to, the sylvite of residual is cleaned with 0.1M HCl, layered porous structure is obtained
Pumpkin derives stratiform carbon material.
2. pumpkin according to claim 1 derives stratiform carbon material as the preparation method of electrode material for super capacitor,
It is characterized in that：The inert gas is argon gas or nitrogen.
3. pumpkin according to claim 1 derives stratiform carbon material as the preparation method of electrode material for super capacitor,
It is characterized in that：The heating rate of the high-temperature calcination is 1-15 DEG C/min.
4. pumpkin according to claim 1 derives stratiform carbon material as the preparation method of electrode material for super capacitor,
It is characterized in that：The inert atmosphere is Ar or N2Atmosphere.
5. pumpkin according to claim 1 derives stratiform carbon material as the preparation method of electrode material for super capacitor,
It is characterized in that：Described layer structure pumpkin derives carbon material, and its specific surface area is more than 2000m2/ g, as ultracapacitor
Electrode material constant current discharge specific capacity under 1A/g is more than 300F/g, and 5000 capacity of constant current charge-discharge are without declining under 10A/g
Subtract.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710311848.XA CN107055530A (en) | 2017-05-05 | 2017-05-05 | Pumpkin derives stratiform carbon as the preparation method of electrode material for super capacitor |
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| CN201710311848.XA CN107055530A (en) | 2017-05-05 | 2017-05-05 | Pumpkin derives stratiform carbon as the preparation method of electrode material for super capacitor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108461755A (en) * | 2018-03-26 | 2018-08-28 | 中国科学技术大学 | A kind of lithium metal battery cathode framework material and preparation method thereof and lithium metal battery cathode |
| CN110668421A (en) * | 2019-10-29 | 2020-01-10 | 江苏科技大学 | Preparation method of biomass porous carbon material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105540585A (en) * | 2016-01-14 | 2016-05-04 | 燕山大学 | Method for preparing electrode material of supercapacitor from mimosa pudica |
| CN105692616A (en) * | 2016-01-14 | 2016-06-22 | 燕山大学 | Method for preparing supercapacitor electrode material from pine needle-base activated carbon material |
| CN105752969A (en) * | 2016-02-29 | 2016-07-13 | 武汉理工大学 | Method for preparing polyatomic self-doped graphene by using natural porous and laminated vegetables |
-
2017
- 2017-05-05 CN CN201710311848.XA patent/CN107055530A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105540585A (en) * | 2016-01-14 | 2016-05-04 | 燕山大学 | Method for preparing electrode material of supercapacitor from mimosa pudica |
| CN105692616A (en) * | 2016-01-14 | 2016-06-22 | 燕山大学 | Method for preparing supercapacitor electrode material from pine needle-base activated carbon material |
| CN105752969A (en) * | 2016-02-29 | 2016-07-13 | 武汉理工大学 | Method for preparing polyatomic self-doped graphene by using natural porous and laminated vegetables |
Non-Patent Citations (1)
| Title |
|---|
| SUYING BAI ET AL: "Pumpkin-Derived Porous Carbon for Supercapacitors with High Perfprmance", 《CHEMISTRY AN ASIAN JOURNAL》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108461755A (en) * | 2018-03-26 | 2018-08-28 | 中国科学技术大学 | A kind of lithium metal battery cathode framework material and preparation method thereof and lithium metal battery cathode |
| CN108461755B (en) * | 2018-03-26 | 2021-05-07 | 中国科学技术大学 | Lithium metal battery negative electrode framework material and preparation method thereof and lithium metal battery negative electrode |
| CN110668421A (en) * | 2019-10-29 | 2020-01-10 | 江苏科技大学 | Preparation method of biomass porous carbon material |
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