CN107240510A - A kind of ZnFe2O4/ C composite nano fiber electrode material for super capacitor and preparation method thereof - Google Patents
A kind of ZnFe2O4/ C composite nano fiber electrode material for super capacitor and preparation method thereof Download PDFInfo
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- CN107240510A CN107240510A CN201710442292.8A CN201710442292A CN107240510A CN 107240510 A CN107240510 A CN 107240510A CN 201710442292 A CN201710442292 A CN 201710442292A CN 107240510 A CN107240510 A CN 107240510A
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- 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
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
-
- 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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- 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 ZnFe2O4Ferric chloride hexahydrate, anhydrous zinc chloride and PAN, are uniformly distributed in DMF solution by/C composite nano fiber electrode material for super capacitor and preparation method thereof by the method for magnetic agitation first, secondly prepare PAN/ZnCl using electrostatic spinning technique2/FeCl3Presoma composite nanometer fiber felt, drying, finally, by the sample after drying be staged through pre-oxidation treatment, Cryogenic air atmosphere calcining, high temperature Ar gas atmosphere calcine three steps be thermally treated resulting in ZnFe2O4/ C composite nano fiber electrode material for super capacitor.ZnFe prepared by this method2O4/ C composite nano fibers are the stable super-fine continuous fibre of frame structure, and diameter control is embedded into the ZnFe in fiber at tens to hundreds of nanometers2O4Nano particle is evenly distributed.This ZnFe2O4/ C composite nano fibers structural stability and good conductivity, energy fast charging and discharging, show excellent chemical property.
Description
Technical field
The present invention relates to field of nano material preparation, and in particular to a kind of ZnFe2O4/ C composite nano fiber ultracapacitors
Electrode material and preparation method thereof.
Background technology
With energy crisis and the continuous deterioration of environmental pollution, the research and development of novel energy-storing material and energy storage device, as working as
The focus of the present research.Ultracapacitor, with its power density it is high, can fast charging and discharging and the features such as have extended cycle life, be considered as
Traditional chemical cell, which can partly be substituted, is used for the traction power source and startup power supply of vehicle.Electrode material is used as ultracapacitor
Emphasis, double layer electrodes material and fake capacitance electrode material can be divided into according to energy storage principle.Metal oxide electrode material
Because having higher electro-chemical activity and electric conductivity, as the fake capacitance electrode material most paid close attention to by scientist.Wherein ternary mistake
Metal oxide is crossed compared to transiton metal binary oxides because being favored with higher specific capacity by numerous researchers.
ZnFe2O4As one kind of ternary transition metal oxide, because nontoxic, cost is low, rich reserves, easily acquisition and excellent oxygen
Change reducing property, cause the interest of vast researcher.
Reported according to numerous researchs, structure nano is to improve the effective method of electrode material chemical property, because
This substantial amounts of research work concentrates on different-shape nano ZnFe2O4The preparation of electrode material.For example, Vadiyar et al.（J.
Mater. Chem. A, 2016,4：3504-3512）Report a kind of ZnFe2O4Nano flower electrode material, when current density is 1
mA/cm2When, specific capacitance is 1625 F/g, when current density is 6 mA/cm2When, specific capacitance is 200 F/g, and its high rate performance is
12.3 %；Selvan et al.（RSC Adv., 2014,4：27022-27029）Report a kind of ZnFe2O4Nano-particle, works as electricity
Current density is 1 mA/cm2When, specific capacitance is 1235 F/g, when current density is 5 mA/cm2When, specific capacitance is 539 F/g, its
High rate performance is 43.6 %.Although scientific research personnel has prepared the good nanometer Zn Fe of specific capacitance performance2O4Electrode material, still
Nanometer Zn Fe2O4Electrode material easily comes off during redox reaction, causes high rate performance and cyclical stability very
Difference, limits its application in ultracapacitor.
Be seen in report on improve ZnFe2O4The method of nanometer material structure stability is a lot, mainly by ZnFe2O4
Nano-particle is combined with carbon, such as Lin et al.（ACS Nano, 2016,10：2728-2735）Prepared using sol-gel process
Go out a kind of ZnFe2O4Nano-particle is uniformly embedded into the composite of continuous carbon net；Zhu et al.（RSC Adv., 2016,6：56069-
56076）A kind of carbon is prepared with reference to porous ZnFe using solvent-thermal method2O4Nanometer ball material.Currently with electrostatic spinning technique system
Standby ZnFe2O4/ C combination electrode materials are rarely found, it is often more important that the diameter for being easier to realize fiber using electrostatic spinning technique can
Control, the advantage such as preparation process is simple, with low cost, can largely produce, by using appropriate collector, can realize fiber
Align, therefore we devise and are staged through pre-oxidation treatment, the calcining of Cryogenic air atmosphere, high temperature Ar gas atmosphere calcining three
The process of step heat treatment prepares ZnFe2O4/ C composite nano fiber electrode material for super capacitor.This material is a kind of one-dimensional
Nano structural material, its advantage is as follows：ZnFe2O4/ C composite nano fibers are super-fine continuous fibre, and diameter control arrives several tens
Hundred nanometers, it is embedded into the ZnFe in fiber2O4Nano particle is evenly distributed, and the introducing of carbon improves electric conductivity, this composite wood
Material has good structural stability, chemical property is got a promotion.
The content of the invention
In order to improve ZnFe2O4The high rate performance and cyclical stability of electrode material, are provided simultaneously with excellent electric conductivity,
The invention provides a kind of ZnFe2O4/ C composite nano fiber electrode material for super capacitor and preparation method thereof, the material conduct
With good high rate performance, electric conductivity and cyclical stability during electrode material for super capacitor.
ZnFe of the present invention2O4The preparation method of/C composite nano fiber electrode material for super capacitor, its step is such as
Under：
（1）Ferric chloride hexahydrate, anhydrous zinc chloride and PAN are uniformly distributed in DMF solvent, magnetic agitation, form forerunner
Body colloidal sol；
（2）By step（1）Obtained precursor sol is placed in the syringe for being connected to high-voltage DC power supply, in default voltage and
Inject and electrostatic spinning is carried out under speed, prepare PAN/ZnCl2/FeCl3Presoma composite nanometer fiber felt, drying；
（3）Sample after drying is staged through pre-oxidation treatment, the calcining of Cryogenic air atmosphere, high temperature Ar gas atmosphere three steps of calcining
It is thermally treated resulting in ZnFe2O4/ C composite nano fiber electrode material for super capacitor.
Step（1）In, the precursor sol, anhydrous zinc chloride is stoichiometrically prepared with ferric chloride hexahydrate, and six
Concentration of the Ferric Chloride Hydrated in DMF solvent is 0.03~0.05 mol/L, more preferably 0.04 mol/L.
Step（1）In, the time of magnetic agitation is 6~15 h, more preferably 10 h.
Step（1）In, anhydrous zinc chloride and PAN mass ratio are 0.01~0.05 in the precursor sol, further
Preferably 0.03.
Step（2）In, a diameter of 0.5~0.7 nm of syringe needle, distance of the syringe needle away from receiver is 14~16
cm。
Step（2）In, the applied voltage of electrostatic spinning is 15~17 kV, injects speed for 0.04~0.1 mm/min.
Step（3）In, the pre-oxidation heat treatment condition is：Pre-oxidation treatment temperature is 250~300 DEG C, soaking time
For 2~4 h.
Step（3）In, the Cryogenic air atmosphere calcination condition is：Calcining heat is 400~500 DEG C, and soaking time is
2~4 h.
Step（3）In, the high temperature Ar gas atmosphere calcination condition is：Calcining heat is 600~800 DEG C, and soaking time is
2~4 h.
Described ZnFe2O4/ C composite nano fiber electrode material for super capacitor, it is characterised in that ZnFe2O4/ C is combined
Nanofiber is the stable super-fine continuous fibre of frame structure, and diameter control is embedded into fiber at tens to hundreds of nanometers
ZnFe2O4Nano particle is evenly distributed.
The beneficial effects of the present invention are：
（1）Preparation method of the present invention is simple and easy to do.
（2）ZnFe2O4/ C composite nano fibers are the stable super-fine continuous fibre of frame structure, and diameter control is arrived tens
Hundreds of nanometers, it is embedded into the ZnFe in fiber2O4Nano particle is evenly distributed.
（3）ZnFe2O4The chemical property of/C composite nano fiber electrode materials be improved significantly.
Brief description of the drawings
Fig. 1 is ZnFe prepared by embodiment 12O4The scanning electron microscope (SEM) photograph of/C composite nano fiber electrode material for super capacitor；
Fig. 2 is ZnFe prepared by embodiment 22O4The scanning electron microscope (SEM) photograph of/C composite nano fiber electrode material for super capacitor；
Fig. 3 is ZnFe prepared by embodiment 32O4The scanning electron microscope (SEM) photograph of/C composite nano fiber electrode material for super capacitor；
Fig. 4 is ZnFe prepared by embodiment 42O4ZnFe prepared by nano-fiber electrode material and embodiment 22O4/ C composite Nanos
When fiber electrode material is made as electrode slice, the constant current charge-discharge curve when current density is 1 A/g.
Embodiment
Technical scheme is further illustrated below by several preferred examples, but described embodiment is said
Bright is only a part of embodiment of the present invention, should not be interpreted as limitation of the present invention in any degree.
Embodiment 1
0.4 mmol ferric chloride hexahydrates, 0.2 mmol anhydrous zinc chlorides, 0.5 g PAN and 10 mL DMF are mixed equal
It is even, solid matter is fully dissolved, obtain precursor sol.Above-mentioned precursor sol is placed into the note for being connected to high-voltage DC power supply
In emitter, pin hole jet diameters are 0.5 nm, and applied voltage is set to 15 kV, injects speed and be set to 0.04 mm/min, open
Beginning electrostatic spinning, prepares PAN/ZnCl2/FeCl3Presoma composite nanometer fiber felt, drying.Sample after drying is placed in pipe
Pre-oxidation treatment, the calcining of Cryogenic air atmosphere, the calcining three steps heat treatment of high temperature Ar gas atmosphere are staged through in formula stove：The first step is pre-
4 h, 5 DEG C/min of heating rate are incubated under oxidizing thermal treatment, 250 DEG C of air atmospheres；Second step Cryogenic air atmosphere is calcined,
400 DEG C of insulations 4 h, 5 DEG C/min of heating rate；Calcined under 3rd step high temperature Ar gas atmosphere, 600 DEG C of 4 h of insulation, heating speed
5 DEG C/min of rate.It is final to collect the ZnFe prepared2O4/ C composite nano fiber electrode material for super capacitor.Its ESEM is such as
Shown in Fig. 1.
Embodiment 2
0.4 mmol ferric chloride hexahydrates, 0.2 mmol anhydrous zinc chlorides, 1 g PAN and 10 mL DMF are mixed equal
It is even, solid matter is fully dissolved, obtain precursor sol.Above-mentioned precursor sol is placed into the note for being connected to high-voltage DC power supply
In emitter, pin hole jet diameters are 0.6 nm, and applied voltage is set to 16 kV, injects speed and be set to 0.07 mm/min
, start electrostatic spinning, prepare PAN/ZnCl2/FeCl3Presoma composite nanometer fiber felt, drying.Sample after drying is put
Pre-oxidation treatment, the calcining of Cryogenic air atmosphere, the calcining three steps heat treatment of high temperature Ar gas atmosphere are staged through in tube furnace：First
3 h, 5 DEG C/min of heating rate are incubated under step pre-oxidation heat treatment, 270 DEG C of air atmospheres；Second step Cryogenic air atmosphere is forged
Burn, 450 DEG C of insulations 3 h, 5 DEG C/min of heating rate；Calcined under 3rd step high temperature Ar gas atmosphere, 700 DEG C of 3 h of insulation, heating
5 DEG C/min of speed.It is final to collect the ZnFe prepared2O4/ C composite nano fiber electrode material for super capacitor.Its ESEM
As shown in Figure 2.
Embodiment 3
0.4 mmol ferric chloride hexahydrates, 0.2 mmol anhydrous zinc chlorides, 1.5 g PAN and 10 mL DMF are mixed equal
It is even, solid matter is fully dissolved, obtain precursor sol.Above-mentioned precursor sol is placed into the note for being connected to high-voltage DC power supply
In emitter, pin hole jet diameters are 0.7 nm, and applied voltage is set to 17 kV, injects speed and be set to 0.1 mm/min, open
Beginning electrostatic spinning, prepares PAN/ZnCl2/FeCl3Presoma composite nanometer fiber felt, drying.Sample after drying is placed in pipe
Pre-oxidation treatment, the calcining of Cryogenic air atmosphere, the calcining three steps heat treatment of high temperature Ar gas atmosphere are staged through in formula stove：The first step is pre-
2 h, 5 DEG C/min of heating rate are incubated under oxidizing thermal treatment, 300 DEG C of air atmospheres；Second step Cryogenic air atmosphere is calcined,
500 DEG C of insulations 2 h, 5 DEG C/min of heating rate；Calcined under 3rd step high temperature Ar gas atmosphere, 800 DEG C of 2 h of insulation, heating speed
5 DEG C/min of rate.It is final to collect the ZnFe prepared2O4/ C composite nano fiber electrode material for super capacitor.Its ESEM is such as
Shown in Fig. 3.
Embodiment 4
ZnFe2O4The ZnFe that the preparation method of nano-fiber electrode material is prepared with embodiment 22O4/ C composite nano fibers are super
The preparation method of capacitor electrode material is consistent, and unique different place is that the calcining of the 3rd step high temperature Ar gas atmosphere is changed to air
Atmosphere is calcined.
By the ZnFe of above-mentioned acquisition2O4ZnFe prepared by nano-fiber electrode material and embodiment 22O4/ C composite Nanos are fine
Electrode slice, sample, conductive black and PVDF Kynoar ethylene glycol solutions is made in dimension electrode material for super capacitor（10 mg/
mL）Mix in proportion, be then coated with nickel foam.Using German Zahner/ZenniumE6.0 electrochemical operation
Stand, in three-electrode system, the electrode slice being made is as working electrode, and Pt is that, to electrode, saturation Ag/AgCl electrodes are reference electricity
Pole, electrolyte is the 2 mol/L KOH aqueous solution, and charging/discharging voltage is -1.1~0 V, at room temperature measuring electrode material constant current
Charge-discharge performance.Capacitive property is more as shown in Figure 4.It can be seen that, ZnFe2O4Nanofiber is carried with the compound rear chemical properties of C
Rise.
Preferred embodiment of the invention described in detail above.It should be appreciated that the ordinary skill of this area is without creative
Work just can make many modifications and variations according to the design of the present invention.Therefore, all technical staff in the art are according to this
The design of invention passes through the available technical side of logical analysis, reasoning, or a limited experiment on the basis of existing technology
Case, all should be in the protection domain being defined in the patent claims.
Claims (9)
1. a kind of ZnFe2O4/ C composite nano fiber electrode material for super capacitor, it is characterised in that ZnFe2O4/ C composite Nanos
Fiber is the stable super-fine continuous fibre of frame structure, and diameter control is embedded into fiber at tens to hundreds of nanometers
ZnFe2O4Nano particle is evenly distributed.
2. ZnFe according to claim 12O4The preparation method of/C composite nano fiber electrode material for super capacitor, it is special
Levy and be, comprise the following steps：
（1）Ferric chloride hexahydrate, anhydrous zinc chloride and PAN are uniformly distributed in DMF solvent by the method for magnetic agitation,
Form precursor sol；
（2）By step（1）Obtained precursor sol is placed in the syringe for being connected to high-voltage DC power supply, in default voltage and
Inject and electrostatic spinning is carried out under speed, prepare PAN/ZnCl2/FeCl3Presoma composite nanometer fiber felt, drying；
（3）Sample after drying is staged through pre-oxidation treatment, the calcining of Cryogenic air atmosphere, high temperature Ar gas atmosphere three steps of calcining
It is thermally treated resulting in ZnFe2O4/ C composite nano fiber electrode material for super capacitor.
3. preparation method as claimed in claim 2, it is characterised in that step（1）In, the precursor sol, six hydration chlorine
Change iron stoichiometrically to prepare with anhydrous zinc chloride, concentration of the ferric chloride hexahydrate in DMF solvent is 0.03~0.05
mol/L。
4. preparation method as claimed in claim 2, it is characterised in that step（1）In, anhydrous chlorination in the precursor sol
Zinc and PAN mass ratio are 0.01~0.05.
5. preparation method as claimed in claim 2, it is characterised in that step（2）In, syringe needle a diameter of 0.5~
0.7 nm, distance of the syringe needle away from receiver is 14~16 cm.
6. preparation method as claimed in claim 2, it is characterised in that step（2）In, the applied voltage of electrostatic spinning for 14~
17 kV, inject speed for 0.02~0.2 mm/min.
7. preparation method as claimed in claim 2, it is characterised in that step（3）In, pre-oxidation heat treatment temperature be 250~
300 DEG C, soaking time is 2~4 h.
8. preparation method as claimed in claim 2, it is characterised in that step（3）In, Cryogenic air atmosphere calcining heat is
400~500 DEG C, soaking time is 2~4 h.
9. preparation method as claimed in claim 2, it is characterised in that step（3）In, high temperature Ar gas atmosphere calcining heats are
600~800 DEG C, soaking time is 2~4 h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106409528A (en) * | 2016-11-11 | 2017-02-15 | 济南大学 | ZnFe2O4-nano-particle/carbon-fiber composite supercapacitor electrode material and preparation method thereof |
| CN111575835A (en) * | 2020-05-15 | 2020-08-25 | 江苏科技大学 | ZnSnO3-C composite nanofiber and preparation method thereof |
| CN114334484A (en) * | 2022-01-05 | 2022-04-12 | 厦门理工学院 | Nickel-copper oxide/carbon composite nanofiber electrode material and preparation method thereof |
| CN114464810A (en) * | 2022-02-16 | 2022-05-10 | 广州大学 | Preparation method and application of sodium ion battery negative electrode material |
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| CN102154739A (en) * | 2010-12-30 | 2011-08-17 | 湘潭大学 | Method for preparing lithium ion battery cathode material ZnFe2O4/C nano fibers |
| CN106409528A (en) * | 2016-11-11 | 2017-02-15 | 济南大学 | ZnFe2O4-nano-particle/carbon-fiber composite supercapacitor electrode material and preparation method thereof |
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2017
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| CN102154739A (en) * | 2010-12-30 | 2011-08-17 | 湘潭大学 | Method for preparing lithium ion battery cathode material ZnFe2O4/C nano fibers |
| CN106409528A (en) * | 2016-11-11 | 2017-02-15 | 济南大学 | ZnFe2O4-nano-particle/carbon-fiber composite supercapacitor electrode material and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106409528A (en) * | 2016-11-11 | 2017-02-15 | 济南大学 | ZnFe2O4-nano-particle/carbon-fiber composite supercapacitor electrode material and preparation method thereof |
| CN111575835A (en) * | 2020-05-15 | 2020-08-25 | 江苏科技大学 | ZnSnO3-C composite nanofiber and preparation method thereof |
| CN111575835B (en) * | 2020-05-15 | 2022-02-11 | 江苏科技大学 | ZnSnO3-C composite nanofiber and preparation method thereof |
| CN114334484A (en) * | 2022-01-05 | 2022-04-12 | 厦门理工学院 | Nickel-copper oxide/carbon composite nanofiber electrode material and preparation method thereof |
| CN114334484B (en) * | 2022-01-05 | 2024-03-12 | 厦门理工学院 | Nickel-copper oxide/carbon composite nanofiber electrode material and preparation method thereof |
| CN114464810A (en) * | 2022-02-16 | 2022-05-10 | 广州大学 | Preparation method and application of sodium ion battery negative electrode material |
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Application publication date: 20171010 |