CN109979762A - A kind of preparation method of porous ferroferric oxide/carbon composite electrode material - Google Patents
A kind of preparation method of porous ferroferric oxide/carbon composite electrode material Download PDFInfo
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- CN109979762A CN109979762A CN201910330462.2A CN201910330462A CN109979762A CN 109979762 A CN109979762 A CN 109979762A CN 201910330462 A CN201910330462 A CN 201910330462A CN 109979762 A CN109979762 A CN 109979762A
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 239000007772 electrode material Substances 0.000 title claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 239000000178 monomer Substances 0.000 claims description 11
- 235000019441 ethanol Nutrition 0.000 claims description 10
- 239000013067 intermediate product Substances 0.000 claims description 10
- 229920000767 polyaniline Polymers 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 239000003643 water by type Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 6
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000005457 ice water Substances 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- 238000002604 ultrasonography Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 2
- -1 Sodium dialkyl sulfate Chemical class 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 239000003990 capacitor Substances 0.000 abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- 239000011258 core-shell material Substances 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000006116 polymerization reaction Methods 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 16
- 239000000463 material Substances 0.000 description 9
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 6
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000011280 coal tar Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 239000002073 nanorod Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- MAQAUGBCWORAAB-UHFFFAOYSA-N [C+4].[O-2].[Fe+2].[O-2].[O-2] Chemical compound [C+4].[O-2].[Fe+2].[O-2].[O-2] MAQAUGBCWORAAB-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 231100000584 environmental toxicity Toxicity 0.000 description 1
- 229940056319 ferrosoferric oxide Drugs 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
- H01G11/46—Metal oxides
-
- 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)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of preparation methods of porous ferroferric oxide/carbon composite electrode material.Porous Fe is prepared with hydro-thermal method3O4, then in Fe3O4On the basis of with oxidizing process polymerization aniline prepare porous core-shell particles Fe3O4/ C composite.The method of the present invention preparation process is simple, reliable, environmentally protective, and obtained ferroferric oxide/carbon composite material has regular space structure, good dispersibility, high-energy density and power density, outstanding cycle performance, it is a kind of ideal electrode material for super capacitor, is especially suitable for industrialized production.
Description
Technical field
The invention belongs to new energy field of material technology, in particular to a kind of porous ferroferric oxide/carbon composite electrode
The preparation method of material.
Background technique
Supercapacitor is due to high-energy density and power density and outstanding cycle performance etc. and as quick
With the primary selection in high-power energy stocking system field.Electrode material in supercapacitor plays the performance of supercapacitor
To vital effect, therefore, realize that the widely applied most important thing of supercapacitor is to prepare and develop high performance electricity
Pole material.
Transition metal oxide and carbon material are the common two kinds of materials of electrode material for super capacitor.Utilize both materials
The advantageous characteristic of material and to overcome deficiency existing for homogenous material to prepare combination electrode material be current electrode material for super capacitor
One of hot spot of research.
The invention proposes a kind of preparation method of porous ferroferric oxide/carbon composite electrode material, supercapacitor with
The features such as its high power density, short charge and discharge time, long circulation life and be concerned, promoting its energy density is currently to need
One of difficult point captured.Many transition metal oxides specific capacity generally with higher, such as RuO2, Fe3O4In metal oxygen
Among compound, ferroso-ferric oxide have the characteristics that it is cheap, without environmental toxicity, Yi Fasheng redox reaction, be considered as pole
Has the electrode material for super capacitor of potentiality.The present invention is prepared for porous Fe by hydro-thermal method3O4/ C composite, passes through
The means such as XRD, FTIR are characterized, it was demonstrated that the pyrolysismethod can synthesize porous Fe really3O4/ C nano composite material.To the material
Carry out cyclic voltammetry, curve approximation rectangle the result shows that the composite material have fake capacitance characteristic.Li et al. proposes one
Kind carbon shell protection scheme, and a kind of iron oxide-carbon nano rod array cathode of binder free is reported, which has preferable
Cyclical stability.It provides high energy and power density, has been more than many flexible super capacitors reported recently.Highest
Energy density values even close to Li hull cell, be several times of 5.5 V/100 mF supercapacitors of business.Especially this is mixed
It attaches together and sets in the case where being significantly bent, mechanical pressure being big, temperature increases (reaching as high as 80 degrees Celsius), be still able to maintain good
Chemical property, environmental suitability is strong.(Li R, Wang Y, Zhou C, et al. Carbon-Stabilized
High‐Capacity Ferroferric Oxide Nanorod Array for Flexible Solid‐State
Alkaline Battery–Supercapacitor Hybrid Device with High Environmental
Suitability [J] Advanced Functional Materials, 2015,25 (33): 5384-5394.).Wang
Chemical activation is carried out to coal-tar residue Deng using potassium hydroxide, then carries out carbonization treatment, is prepared for that there is tridimensional network
Oxygen-enriched active carbon.Nanostructure Fe is prepared for using simple chemical coprecipitation3O4/ AC composite material, as supercapacitor
Active electrode material.With pure Fe3O4It is compared with AC, Fe3O4Significantly improving for/AC nanocomposite chemical property can close
Reason ground is attributed to Fe3O4Positive synergistic effect between AC.(Wang Y, He P, Zhao X, et al. Coal
tar residues-based nanostructured activated carbon/Fe3O4 composite electrode
materials for supercapacitors[J]. Journal of Solid State Electrochemistry,
2014,18 (3): 665-672.).
Therefore high-performance super capacitor electrode material is prepared for it in electrochemical energy storage using simple synthetic technology
The application in field is of great significance.The present invention is with FeCl3It is raw material with aniline, porous core-shell particles is prepared using hydro-thermal method
Fe3O4/ C composite.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of porous ferroferric oxide/carbon composite electrode material.
Thinking of the present invention: porous Fe is prepared with hydro-thermal method3O4, then in Fe3O4On the basis of polymerization aniline prepare it is porous
Core-shell particles Fe3O4/ C composite.
Specific steps are as follows:
(1) by 2.03 g Fe3O4·6H2O、1.85 g CH3COONa and 0.09 g Nano-meter SiO_22It is dissolved in 50 mL solvents,
30 min of magnetic agitation, is allowed to form uniform clear solution, then heats 8 h in 180 DEG C of reaction kettles, is cooled to room temperature
Afterwards, it with deionized water and ethanol washing, is finally dried at 80 DEG C, intermediate product is made.
(2) the HF solution that intermediate product mass percent concentration made from step (1) is 2% is impregnated into 60 min, then
It is cleaned 6 times with deionized water, it is finally dry at 80 DEG C, porous Fe is made3O4。
(3) porous Fe made from 0.5 g step (2) is taken3O4It is dissolved in 40 mL deionized waters, 30 min of ultrasound add
0.1g lauryl sodium sulfate, stirs evenly, and adds 0.5 ~ 2mL aniline monomer, 20 min is stirred under the conditions of ice-water bath, dropwise
It is added and contains 3.1 ~ 12.4 g FeCl3FeCl3Solution reacts 3 h, and Magneto separate goes out magnetic substance, with ethyl alcohol and deionization
Water washing, products therefrom is dry at 80 DEG C, obtains Fe3O4/ PANI presoma.
(4) by Fe made from step (3)3O4/ PANI presoma is heated to 600 under Ar atmosphere with the rate of 3 DEG C/min
DEG C heat preservation 3 h, obtain porous ferroferric oxide/carbon composite electrode material.
The solvent is the mixture of ethylene glycol or deionized water or both.
The method of the present invention preparation process is simple, reliable, environmentally protective, and obtained ferroferric oxide/carbon composite material has
There are regular space structure, good dispersibility, high-energy density and power density, outstanding cycle performance, is a kind of ideal
Electrode material for super capacitor, be especially suitable for industrialized production.
Specific embodiment
Embodiment 1:
(1) by 2.03 g Fe3O4·6H2O、1.85 g CH3COONa and 0.09 g Nano-meter SiO_22It is dissolved in 33 mL ethylene glycol
In 17 mL deionized waters, 30 min of magnetic agitation is allowed to form uniform clear solution, then in 180 DEG C of reaction kettles
8 h are heated, after being cooled to room temperature, with deionized water and ethanol washing, is finally dried at 80 DEG C, intermediate product is made.
(2) the HF solution that intermediate product mass percent concentration made from step (1) is 2% is impregnated into 60 min, then
It is cleaned 6 times with deionized water, it is finally dry at 80 DEG C, porous Fe is made3O4。
(3) porous Fe made from 0.5 g step (2) is taken3O4It is dissolved in 40 mL deionized waters, 30 min of ultrasound add
0.1g lauryl sodium sulfate, stirs evenly, and adds 1 mL aniline monomer, stirs 20 min under the conditions of ice-water bath, dropwise plus
Enter to contain 6.2 g FeCl3FeCl3Solution reacts 3 h, and Magneto separate goes out magnetic substance, washed with ethyl alcohol and deionized water,
Products therefrom is dry at 80 DEG C, obtains Fe3O4/ PANI presoma.
(4) by Fe made from step (3)3O4/ PANI presoma is heated to 600 under Ar atmosphere with the rate of 3 DEG C/min
DEG C heat preservation 3 h, obtain porous ferroferric oxide/carbon composite electrode material.
Embodiment 2:
(1) by 2.03 g Fe3O4·6H2O、1.85 g CH3COONa and 0.09 g Nano-meter SiO_22It is dissolved in 25 mL ethylene glycol
In 25 mL deionized waters, 30 min of magnetic agitation is allowed to form uniform clear solution, then in 180 DEG C of reaction kettles
8 h are heated, after being cooled to room temperature, with deionized water and ethanol washing, is finally dried at 80 DEG C, intermediate product is made.
(2) the HF solution that intermediate product mass percent concentration made from step (1) is 2% is impregnated into 60 min, then
It is cleaned 6 times with deionized water, it is finally dry at 80 DEG C, porous Fe is made3O4。
(3) porous Fe made from 0.5 g step (2) is taken3O4It is dissolved in 40 mL deionized waters, 30 min of ultrasound add
0.1g lauryl sodium sulfate, stirs evenly, and adds 1 mL aniline monomer, stirs 20 min under the conditions of ice-water bath, dropwise plus
Enter to contain 6.2 g FeCl3FeCl3Solution reacts 3 h, and Magneto separate goes out magnetic substance, washed with ethyl alcohol and deionized water,
Products therefrom is dry at 80 DEG C, obtains Fe3O4/ PANI presoma.
(4) by Fe made from step (3)3O4/ PANI presoma is heated to 600 under Ar atmosphere with the rate of 3 DEG C/min
DEG C heat preservation 3 h, obtain porous ferroferric oxide/carbon composite electrode material.
Embodiment 3:
(1) by 2.03 g Fe3O4·6H2O、1.85 g CH3COONa and 0.09 g Nano-meter SiO_22It is dissolved in 50 mL ethylene glycol
In, 30 min of magnetic agitation is allowed to form uniform clear solution, then heats 8 h in 180 DEG C of reaction kettles, is cooled to room
Wen Hou is finally dried at 80 DEG C with deionized water and ethanol washing, and intermediate product is made.
(2) the HF solution that intermediate product mass percent concentration made from step (1) is 2% is impregnated into 60 min, then
It is cleaned 6 times with deionized water, it is finally dry at 80 DEG C, porous Fe is made3O4。
(3) porous Fe made from 0.5 g step (2) is taken3O4It is dissolved in 40 mL deionized waters, 30 min of ultrasound add
0.1g lauryl sodium sulfate, stirs evenly, and adds 1 mL aniline monomer, stirs 20 min under the conditions of ice-water bath, dropwise plus
Enter to contain 6.2 g FeCl3FeCl3Solution reacts 3 h, and Magneto separate goes out magnetic substance, washed with ethyl alcohol and deionized water,
Products therefrom is dry at 80 DEG C, obtains Fe3O4/ PANI presoma.
(4) by Fe made from step (3)3O4/ PANI presoma is heated to 600 under Ar atmosphere with the rate of 3 DEG C/min
DEG C heat preservation 3 h, obtain porous ferroferric oxide/carbon composite electrode material.
Embodiment 4:
The step of repeating embodiment 1, the additional amount for only changing the step aniline monomer in (5) is 0.5 mL and FeCl3Solution (contains
3.1 g FeCl3).
Embodiment 5:
The step of repeating embodiment 1, the additional amount for only changing the step aniline monomer in (5) is 2 mL and FeCl3Solution (contains 12.4
g FeCl3).
Embodiment 6:
The step of repeating embodiment 2, the additional amount for only changing the step aniline monomer in (5) is 0.5 mL and FeCl3Solution (contains
3.1 g FeCl3).
Embodiment 7:
The step of repeating embodiment 2, the additional amount for only changing the step aniline monomer in (5) is 2 mL and FeCl3Solution (contains 12.4
g FeCl3).
Embodiment 8:
The step of repeating embodiment 3, the additional amount for only changing the step aniline monomer in (5) is 0.5 mL and FeCl3Solution (contains
3.1 g FeCl3).
Embodiment 9:
The step of repeating embodiment 2, the additional amount for only changing the step aniline monomer in (5) is 2 mL and FeCl3Solution (contains 12.4
g FeCl3).
Claims (1)
1. a kind of preparation method of porous ferroferric oxide/carbon composite electrode material, it is characterised in that specific steps are as follows:
(1) by 2.03 g Fe3O4·6H2O、1.85 g CH3COONa and 0.09 g Nano-meter SiO_22It is dissolved in 50 mL solvents,
30 min of magnetic agitation, is allowed to form uniform clear solution, then heats 8 h in 180 DEG C of reaction kettles, is cooled to room temperature
Afterwards, it with deionized water and ethanol washing, is finally dried at 80 DEG C, intermediate product is made；
(2) the HF solution that intermediate product mass percent concentration made from step (1) is 2% is impregnated into 60 min, then spent
Ionized water cleans 6 times, finally dry at 80 DEG C, and porous Fe is made3O4；
(3) porous Fe made from 0.5 g step (2) is taken3O4It is dissolved in 40 mL deionized waters, 30 min of ultrasound add 0.1g ten
Sodium dialkyl sulfate stirs evenly, and adds 0.5 ~ 2mL aniline monomer, 20 min are stirred under the conditions of ice-water bath, is added dropwise and contains
3.1~12.4 g FeCl3FeCl3Solution reacts 3 h, and Magneto separate goes out magnetic substance, washed with ethyl alcohol and deionized water,
Products therefrom is dry at 80 DEG C, obtains Fe3O4/ PANI presoma；
(4) by Fe made from step (3)3O4/ PANI presoma is heated to 600 DEG C of guarantors under Ar atmosphere with the rate of 3 DEG C/min
3 h of temperature, obtain porous ferroferric oxide/carbon composite electrode material；
The solvent is the mixture of ethylene glycol or deionized water or both.
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2019
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Application publication date: 20190705 |