CN109961966A - Peanut shell porous carbon/ferroso-ferric oxide combination electrode material preparation method - Google Patents
Peanut shell porous carbon/ferroso-ferric oxide combination electrode material preparation method Download PDFInfo
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- CN109961966A CN109961966A CN201711452761.0A CN201711452761A CN109961966A CN 109961966 A CN109961966 A CN 109961966A CN 201711452761 A CN201711452761 A CN 201711452761A CN 109961966 A CN109961966 A CN 109961966A
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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
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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
- H01G11/46—Metal oxides
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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 invention discloses a kind of novel preparation methods of peanut shell porous carbon/ferroso-ferric oxide combination electrode material, and introduce its application in terms of electrode of super capacitor.With peanut shell, FeKMnO4As raw material, large specific surface area is prepared using ultrasonic treatment and high temperature cabonization processing, the composite material of superior performance, ferroferric oxide nano-piece size is between 500nm-700nm.The nanometer sheet of carbon material surface growth not only increases material specific surface area, while providing certain fake capacitance, considerably increases material capacitive property.In addition, the preparation method is easy to operate, environmental protection, at low cost, the waste recycling in life is turned waste into wealth in easily controllable and scale.
Description
Technical field
The present invention relates to a kind of preparation methods of electrode material for super capacitor, are based especially on the more of biomass peanut shell
The novel preparation method of hole carbon composite electrode material.This method is easy to operate, at low cost, reproducible, and easily controllable.
Background technique
The increase of demand with the mankind to cleaning sustainable energy, electric chemical super capacitor is because power density is high, follows
The ring service life is long, has become one of main emerging energy storage device using the advantages such as safe.But low energy densities are them in energy storage
The main obstacle of field practical application.In order to improve energy density, many research concern exploitations have the green wood of high specific capacitance
Material and the unsymmetric structure system with wider operating voltage window.
In electric double layer type capacitor electrode material, the characteristics of carbon material is due to abundant raw materials, clean and environmental protection, using most
To be extensive, while its production technology is also increasingly mature.Active carbon is most commonly seen in current commercial supercapacitor.However, living
Property Carbon Materials itself due to the problems such as there are size distribution is uneven, electrolyte and electrode material cannot be come into full contact with.Reason
The carbon material thought should meet: the specific surface area with superelevation, reasonable Kong Rong and pore-size distribution, good electric conductivity and wet
Lubricant nature, material surface are preferably present the active material that fake capacitance reaction can occur other than it can generate electric double layer capacitance.
China is large agricultural country, there is a large amount of shell and timber every year.Wherein, peanut shell is as daily life waste,
If its active carbon for preparing high electrochemical performance can be utilized, peanut shell will have good application value, turn waste into wealth.
The present invention introduces special high-valence state metal ion using potassium ferrate solution, then direct pyrocarbon using peanut shell as raw material
Change, the porous carbon/ferroso-ferric oxide combination electrode material haveing excellent performance is prepared.By controlling potassium ferrate solution concentration,
The pattern of adjustable ferriferrous oxide nano structure, to optimize the energy-storage property of electrode.
Summary of the invention
The purpose of the present invention: propose that one kind using biological fiber waste as raw material, utilizes strong oxidizer potassium ferrate solution
Peanut shell is handled in conjunction with the method for ultrasound, potassium ferrate introduces special high-valence state metal ion simultaneously, then direct high temperature
Porous carbon/ferroso-ferric oxide the combination electrode material haveing excellent performance is prepared in carbonization.The present invention is directed to will be in daily life
Waste peanut shell is turned waste into wealth, and good application value is made it have；And overcome the defect of the low capacitor of single carbon material, it is maximum
Degree optimizes porous carbon/ferriferrous oxide composite material specific capacitance.
1, the technical scheme is that clean, structural integrity peanut shell is cut into fragment by surface, and mechanical lapping at
It is powdered, absolute ethyl alcohol and stirring is added to uniform, then ultrasonic disperse 10min, is washed with deionized clean；Take suitable flower
Raw shell powder is added to certain density FeKMnO4In solution, ultrasonic disperse 30min, next by aaerosol solution stand 6h with
On；Pretreated peanut shell powder is cleaned repeatedly with deionized water, is then placed in 80 DEG C of vacuum oven drying；After dry
Powder be put into vacuum tube furnace, a certain temperature within the scope of 600~900 DEG C is heated to 5 DEG C/min in argon atmosphere, and
2h carries out carbonization treatment under this steady temperature atmosphere, obtains final product.
Before handling peanut shell, clean, structural integrity the peanut shell by surface is needed to be cut into fragment, and mechanical grinding
It clays into power shape, it is made to be easier to infiltrate in subsequent processing, absolute ethyl alcohol and stirring is then added to uniform, then ultrasonic disperse
Clean, drying is washed with deionized in 10min.
As preferred plan, peanut shell powder is in FeKMnO4Concentration range 20g/L~25g/L, FeKMnO in solution4It is molten
Liquid concentration range is 1~5M.
As preferred plan, by FeKMnO4The peanut shell powder of solution suspension dispersion ultrasonic disperse under 100W power
30min；
As preferred plan, the aaerosol solution after ultrasonic treatment is stood into 6h or more；
As preferred plan, pretreated peanut shell powder is cleaned repeatedly with deionized water, is then placed in vacuum drying
80 DEG C of case drying, temperature are 80 DEG C, and drying time is 2h or more.
As preferred plan, the powder after drying is put into vacuum tube furnace, is added under inert gas protection with 5 DEG C/min
A certain temperature within the scope of heat to 600~900 DEG C, and 2h carries out carbonization treatment under this steady temperature atmosphere.
Obtained peanut shell porous carbon/ferroso-ferric oxide can be applied to electrode material for super capacitor.The present invention is for the first time
This composite material based on activated carbon from activated sludge and nano-metal-oxide, electrochemical performance is made.With other methods
It compares, preparation method proposed by the present invention is not necessarily to any template, at low cost, environmentally friendly and easily controllable and scale.
Beneficial effects of the present invention:
(1) the invention proposes the composite materials and one of a kind of biomass porous carbon-supported metal oxide nanostructure
Footwork preparation method.
(2) peanut shell porous carbon can be prepared by only relying on strong oxidizer surface treatment, physical means ultrasound and heat treatment
Load the combination electrode material of ferriferrous oxide nano structure.
(3) compared with other methods, which has following particular advantages:
1. experimental provision, experiment condition and preparation process are very simple, easy to operate；
2. controllability is good, the pattern and nanostructure of ferroso-ferric oxide are controlled by adjusting concentration realization；
3. it is low in cost, there is good industrial applications prospect；
4. strong applicability can be generalized to the preparation of other activated carbon from activated sludge/nano metal oxide composite materials.
Detailed description of the invention
Fig. 1 is the picture of material preparation process.(a) primary peanut shell and peanut shell coatings；(b) it 1. is just added
FeKMnO4Solution；2. ultrasonic reaction 30min；3. drying product after processing；4. final product after carbonization.
Fig. 2 is SEM and the TG figure that product is made in embodiment 1-5.FeKMnO4The concentration of solution is respectively (a) 1M；(b)2M；
(c)3M；(d)4M；(e)5M；(f) various concentration FeKMnO4The TG figure of product is made in solution
Fig. 3 is using 3M FeKMnO4The different amplification SEM figure of product is made in solution (embodiment 3).
Fig. 4 is the XRD diagram that embodiment 1-5 prepares electrode material.
Fig. 5 is the EDS figure that embodiment 3 prepares electrode material.
Fig. 6 is the electrochemical property test figure of the Different electrodes material of embodiment 1-5 preparation.Various concentration FeKMnO4System
Obtain material (a) CV curve；(b) CD curve；The 3M FeKMnO of optimization4(c) CV curve of material is made in solution；(d) CD curve.
Fig. 7 is the high rate performance figure and 3M FeKMnO that embodiment 1-5 prepares electrode material4The circulation of material is made in solution
Performance map.
Specific embodiment
The peanut shell base for being supported with metal oxide nanostructure is successfully prepared using the method for high temperature cabonization in the present invention
The specific embodiment of porous carbon super capacitor material is as follows:
Embodiment 1
The preparation of peanut shell Quito mesoporous activated carbon material: by surface, clean, structural integrity peanut shell is cut into fragment, and mechanical
It is ground into powder, absolute ethyl alcohol and stirring is added to uniform, then the ultrasonic disperse 10min under 100W power, uses deionized water
Washes clean, drying；Suitable peanut shell powder is taken to be added to the FeKMnO of 1M4In solution, then in ultrasonic reactor
Ultrasonic disperse 30min under 100W power；Next aaerosol solution is stood into 6h；With deionized water by pretreated peanut shell powder
It cleans repeatedly, is then placed in 80 DEG C of vacuum oven drying；Powder after drying is put into vacuum tube furnace, argon atmosphere with
5 DEG C/min is heated to 800 DEG C, and 2h carries out carbonization treatment under this steady temperature atmosphere, obtains final product.
Fig. 1 a is peanut shell and peanut shell coatings in 1 preparation process of embodiment, and primary peanut shell powder is in khaki.Figure
1b is the procedure chart and carbonized product figure of potassium ferrate processing peanut shell in 1 preparation process of embodiment, in which: 1. are just added
FeKMnO4After solution, it can be seen that dispersion liquid is in crocus；2. dispersion liquid is in isabelline after 30min ultrasound；3. passing through
FeKMnO4After the peanut shell powder of processing is dry, powder becomes crocus；4. product is in black powder after carbonization.
Embodiment 2
FeKMnO4The concentration of solution is 2M, and other conditions and embodiment 1 are identical.
Embodiment 3
FeKMnO4Solution concentration is 3M, and other conditions and embodiment 1 are identical.
Embodiment 4
FeKMnO4Solution concentration is 4M, and other conditions and embodiment 1 are identical.
Embodiment 5
FeKMnO4Solution concentration is 5M, and other conditions and embodiment 1 are identical.
As can be seen that the material surface after carbonization has born lamellar structure or chondritic in Fig. 2, (implement in a-c
Example 1-3), in low concentration, laminated structure gradually increases, fine and close；(embodiment 4-5) can see from d-e, and concentration continues
Increase, carbon surface has grown chondritic, and concentration continues to increase, and chondritic increases, and agglomerates blocking；F figure is embodiment 1-5
The thermal multigraph of product is made, surfacing quality accounting is successively are as follows: 5%, 11%, 13.3%, 17%, 19.4%.
Fig. 3 is optimization concentration 3M FeKMnO4The SEM figure under the different amplification of material is made in solution (embodiment 3).
As can be seen that material surface grows the flaky nanometer structure of even compact, the size of nanometer sheet between 500nm-700nm,
These laminated structures significantly increase the specific surface area of material, and active ferroso-ferric oxide is fake capacitance energy storage characteristic, to increase
The specific capacitance of strong composite material.
Fig. 4 is various concentration FeKMnO4The XRD diagram of material is made in solution (embodiment 1-5).It can be seen that at 43.37 °,
57.4 °, 63.1 ° have apparent diffractive features peak, and no other obvious miscellaneous peaks occur, and illustrate that the product component of surface growth is
Fe3O4。
Fig. 5 is optium concentration 3M FeKMnO4The EDS figure of material is made in solution.From this three figures as can be seen that material table
Fe, O element in face distribute very evenly, their atomic ratios are Fe: O=43: 56, close to 3: 4.
Embodiment 6
After carbonized product takes out, acetylene black and PTFE are added with 7: 2: 1 ratio respectively, a small amount of ethyl alcohol is added and is ground in agate
It is ground in alms bowl uniformly until film-form, after being pressurizeed with glass bar, is cut into the rectangular shaped sheet having a size of 2cm × 1cm, then pressed
In nickel foam；The nickel foam substrate used is rectangle, size 2cm × 1cm, convenient for the test of capacitive property.
Fig. 6 a is various concentration FeKMnO4The cyclic voltammetry curve for the material that solution (embodiment 1-5) obtains, sweep speed
For 10mVs-1.It can be seen from the figure that CV curve all deviates rectangle to a certain extent, this is because the electrode charge and discharge process is deposited
In fake capacitance behavior；Under identical sweep speed, the CV curve surround the area of peanut shell carbon material is minimum, and optium concentration 3M
FeKMnO4The area that the CV curve that material is made in solution surrounds is maximum.Compared with pure peanut shell carbon material, the ratio electricity of composite material
Rong Douyou is obviously improved.Fig. 6 b is various concentration FeKMnO4The constant current charge-discharge curve for the material that solution obtains, current density are
0.5Ag-1；Symmetrical Triangle-Profile is all presented in charging and discharging curve, and slope is held essentially constant, and illustrates that material has good electricity
Hold characteristic.By being calculated, under identical current density, the specific capacitance highest of composite material prepared by embodiment 3.Fig. 6 c
It is respectively the cyclic voltammetry curve and charging and discharging curve for optimizing composite material with Fig. 6 d, in 0.5A g-1Under current density, material
Specific capacitance is 260F/g.
Fig. 7 a is various concentration FeKMnO4The high rate performance for the material that solution (embodiment 1-5) obtains.As seen from the figure,
After introducing potassium ferrate solution, the whole specific capacitance of material has very big promotion, and is also able to maintain at higher current densities higher
Specific capacitance；Fig. 7 b is the cycle performance figure that composite material is made in embodiment 3, it can be seen that passes through 5000 charge and discharge cycles
Afterwards, the capacitor of material stills remain in 82% or more, shows that the combination electrode material has good cyclical stability.
Claims (7)
1. a kind of porous carbon based on peanut shell/ferroso-ferric oxide hybrid supercapacitor electrode material preparation method, special
Sign is, by surface, clean, structural integrity peanut shell is cut into fragment, and mechanical lapping is added dehydrated alcohol and stirs at powdered
It mixes to uniform, then ultrasonic disperse 10min, is washed with deionized clean；Suitable peanut shell powder is taken to be added to certain dense
The FeKMnO of degree4In solution, next aaerosol solution is stood 6h or more by ultrasonic disperse 30min；It will be pre-processed with deionized water
Peanut shell powder afterwards is cleaned repeatedly, is then placed in 80 DEG C of vacuum oven drying；Powder after drying is put into vacuum tube furnace
In, a certain temperature within the scope of 600~900 DEG C is heated to 5 DEG C/min under inert gas protection, and in this steady temperature gas
2h carbonization treatment is carried out under atmosphere, obtains final product.
2. preparation method according to claim 1, which is characterized in that before handling peanut shell, need surface
Completely, the peanut shell of structural integrity is cut into fragment, and mechanical lapping makes it be easier to infiltrate in subsequent processing at powdered,
Then absolute ethyl alcohol and stirring is added to uniform, then ultrasonic disperse 10min, is washed with deionized clean, drying.
3. preparation method according to claim 1, which is characterized in that suitable peanut shell powder is taken to be added to FeKMnO4It is molten
It is surface-treated in liquid, the concentration range of peanut shell powder in the solution is 20g/L~25g/L, FeKMnO4Solution concentration model
It encloses for 1~5M.
4. preparation method according to claim 1, which is characterized in that by FeKMnO4The peanut shell powder of solution suspension dispersion
The ultrasonic disperse 30min under 100W power；Aaerosol solution after ultrasonic treatment is stood into 6h or more.
5. preparation method according to claim 1, which is characterized in that with deionized water that pretreated peanut shell powder is anti-
Multiple cleaning, is then placed in vacuum oven and dries, and temperature is 80 DEG C, and drying time is 2h or more.
6. preparation method according to claim 1, which is characterized in that the powder after drying is put into vacuum tube furnace,
The a certain temperature within the scope of 600~900 DEG C is heated to 5 DEG C/min under inert gas shielding, and under this steady temperature atmosphere
It is carbonized, time 2h.
7. peanut shell porous carbon/ferroso-ferric oxide obtained by can be applied to electrode material for super capacitor.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112735857A (en) * | 2020-12-22 | 2021-04-30 | 上海卓笙环保科技有限公司 | Method for constructing composite material based on bean sprouts |
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