CN107658143B - A kind of ferrocenyl supercapacitor - Google Patents
A kind of ferrocenyl supercapacitor Download PDFInfo
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- CN107658143B CN107658143B CN201710878755.5A CN201710878755A CN107658143B CN 107658143 B CN107658143 B CN 107658143B CN 201710878755 A CN201710878755 A CN 201710878755A CN 107658143 B CN107658143 B CN 107658143B
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Abstract
The present invention discloses a kind of ferrocenyl supercapacitor, and the ferrocenyl supercapacitor includes working electrode, reference electrode and to electrode and electrolyte, wherein the working electrode is prepared using ferrocenyl carbon nanotube.The present invention redox characteristic and hydrophily splendid using ferrocenyl carbon nanotube, can be used as the electrode material of supercapacitor, a kind of Novel super capacitor are made, to greatly improve the chemical property of supercapacitor.
Description
Technical field
The present invention relates to supercapacitor technologies field more particularly to a kind of ferrocenyl supercapacitors.
Background technique
Supercapacitor (Supercapacitors, abbreviation SCs) is used as a kind of high-power compensation and energy storage device, both has
There are quick charging and discharging capabilities, long circulation life that there is high security again, is a kind of new and effective energy storage device.Carbon nanotube is made
For a kind of common carbon-based material, it is widely used in supercapacitor.But the specific surface area of usual carbon nanotube is lower,
It is generally less than 100Fg as the specific capacitance of electrode material for electric double layer capacitor-1, and efficiency for charge-discharge is not high, exists and puts certainly
Electrical phenomena, easy to reunite etc. cannot meet actual demand very well.So needing to carry out modification to carbon nanotube, its electricity is improved
Chemical property.
Ferrocene is a kind of metal organic complex with pi bond type interlayer structure, special with splendid redox
Property, therefore ferrocene derivatives are often prepared into modified electrode for developing electrochemistry and bio-sensing as redox matrix
Device.
Summary of the invention
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of ferrocenyl supercapacitor, purports
Existing carbon nanotube is being solved as electrode material for super capacitor, the lower problem of chemical property.
Technical scheme is as follows:
A kind of ferrocenyl supercapacitor, including working electrode, reference electrode and to electrode and electrolyte, wherein institute
It states working electrode to be prepared using ferrocenyl carbon nanotube (CNT-COFc), the chemistry knot of the ferrocenyl carbon nanotube
Structure formula is as follows:
The ferrocenyl supercapacitor, wherein the preparation method of the working electrode is comprising steps of weigh two cyclopentadienyls
Iron-based carbon nanotube adds bonding agent and conductive agent, is tuned into paste, is pressed together on carrier, toasts and ferrocenyl carbon nanometer is made
Pipe electrode.
The ferrocenyl supercapacitor, wherein the preparation method of the working electrode specifically includes step:
The ferrocenyl carbon nanotube for weighing 5mg, adds the bonding agent of 1mg and the conductive agent of 1mg, is tuned into paste, pressing
10h is toasted on carrier, at 100 DEG C, and ferrocenyl carbon nanotube electrode is made.
The ferrocenyl supercapacitor, wherein the bonding agent is 60wt% polytetrafluoroethyl-ne aqueous solution.
The ferrocenyl supercapacitor, wherein the conductive agent is acetylene black.
The ferrocenyl supercapacitor, wherein the carrier is foam nickel sheet.
The ferrocenyl supercapacitor, wherein the size of the foam nickel sheet is 1cm × 5cm.
The ferrocenyl supercapacitor, wherein the reference electrode is Ag/AgCl, and described is Pt to electrode,
The electrolyte is Na2SO4。
The utility model has the advantages that ferrocenyl carbon nanotube of the present invention has splendid redox characteristic and hydrophily,
As electrode material for super capacitor, the chemical property of supercapacitor can be greatly improved.
Detailed description of the invention
Fig. 1 is the synthetic reaction formula of CNT-COFc in embodiment 1.
Fig. 2 is TG comparison diagram of the CNT and CNT-COFc in dry air atmosphere in embodiment 1.
Fig. 3 A is viewgraph of cross-section of the water droplet on CNT (A) in embodiment 1.
Fig. 3 B is viewgraph of cross-section of the water droplet on CNT-COFc (B) in embodiment 1.
The SEM figure that Fig. 4 A is CNT (A) in embodiment 1.
The SEM figure that Fig. 4 B is CNT-COFc (B) in embodiment 1.
Fig. 5 is CNT and CNT-COFc in embodiment 1 in 10mVs-1CV figure.
Fig. 6 is CNT and CNT-COFc in embodiment 1 in 10mVs-1Specific capacitance comparison diagram.
Fig. 7 is CV figure of the CNT-COFc under different scanning rates in embodiment 1.
The specific capacitance that Fig. 8 is CNT-COFc in embodiment 1 is with the trend chart of sweep speed.
The constant current charge-discharge curve that Fig. 9 is CNT-COFc under different current densities in embodiment 1.
Dependence schematic diagram of the specific capacitance to current density that Figure 10 is CNT-COFc in embodiment 1.
Figure 11 is that current density is 2Ag in embodiment 1-1When CNT-COFc specific capacitance conservation rate to cycle-index according to
Rely property schematic diagram.
Specific embodiment
The present invention provides a kind of ferrocenyl supercapacitor, to make the purpose of the present invention, technical solution and effect more
Clear, clear, the present invention is described in more detail below.It should be appreciated that specific embodiment described herein is only used to
It explains the present invention, is not intended to limit the present invention.
The present invention provides a kind of ferrocenyl supercapacitor, including working electrode, reference electrode and to electrode, and electrolysis
Matter, wherein the working electrode is prepared using ferrocenyl carbon nanotube, the chemistry knot of the ferrocenyl carbon nanotube
Structure formula is as follows:
Ferrocenyl carbon nanotube of the present invention has splendid redox characteristic and hydrophily, as super electricity
Container electrode material can greatly improve the chemical property of supercapacitor.
Specifically, the preparation method of the working electrode adds bonding agent comprising steps of weigh ferrocenyl carbon nanotube
And conductive agent, it is tuned into paste, is pressed together on carrier, toasts and ferrocenyl carbon nanotube electrode is made.
Below by embodiment, the present invention is described in detail.
Embodiment
1, reagent
Highly conductive multi-walled carbon nanotube CNT is purchased from Suzhou Tan Feng graphene Science and Technology Ltd., directly uses.Anhydrous chlorination
Aluminium (purity > 99%), oxalyl chloride (purity > 98%), ferrocene (purity > 99%) are purchased from MACKLIN company, directly make
With.Concentrated nitric acid, potassium permanganate, perchloric acid, citric acid, hydrochloric acid, tetrahydrofuran, analysis is pure, is purchased from Guangzhou Chemical Reagent Factory, directly
It uses.Methylene chloride, analysis is pure, is purchased from Guangzhou Chemical Reagent Factory, and calcium hydride water removal is spare.Nickel foam, ptfe emulsion,
Source battery sales department purchased from Taiyuan Yingze District power.All experimental waters are Millipore ultrapure water.
2, the preparation of CNT-COFc
The specific synthetic reaction formula of CNT-COFc is as shown in Figure 1.Carboxylic carbon nano-tube (CNT-COOH) is according to literature method
It synthesizes (Chem.Mater.2004,16:2174-2179), specifically disperses dense nitre for highly conductive multi-walled carbon nanotube (CNT)
In the mixed liquors of acid, potassium permanganate and perchloric acid, ultrasound 7 hours in superpower Ultrasound Instrument are placed in, are washed and dried after taking-up,
Obtain carboxylic carbon nano-tube (CNT-COOH).1.5 grams of carboxylic carbon nano-tubes (CNT-COOH) are weighed, dry three are added to
In mouth bottle, 40 milliliters of anhydrous methylene chlorides are added, under argon gas protection, 1 milliliter of oxalyl chloride is added to 3 degree, with syringe in ice bath, low
3 degree of temperature are reacted 1 hour, then reacted at room temperature 10 hours.Decompression extracts unreacted oxalyl chloride and solvent, under argon gas protection, then plus
Enter 2.3 grams of anhydrous aluminum chlorides and 50 milliliters of anhydrous methylene chlorides, stirs 10 minutes, 1.2 grams of ferrocene are added to 3 degree in ice bath, low
3 degree of temperature are reacted 1 hour, and room temperature reaction is reacted 2 hours again under 4 hours, 40 degree.30 milliliters of 5molL are slowly added dropwise-1Hydrochloric acid it is whole
It only reacts, filters, alternately wash filter cake with tetrahydrofuran and dilute hydrochloric acid, remove aluminium chloride and unreacted ferrocene.Product 40
Degree vacuum drying, obtains 1.7 grams of ferrocenyl carbon nanotubes (CNT-COFc).
3, the preparation of CNT-COFc working electrode
The preparation method of working electrode: weighing CNT-COFc 5mg, adds glue (the 60wt% polytetrafluoroethylene (PTFE) cream of 1mg
Liquid) and 1mg acetylene black, be tuned into paste, be pressed together on foam nickel sheet (being cut into 1cm × 5cm), 100 DEG C of baking 10h are made
CNT-COFc working electrode.
4, test and characterization
Thermogravimetric analysis (TG) is measured using PerkinElmer TGA 8000, and work atmosphere is dry air, heating rate
It is 10 degrees/min.The inductively coupled plasma of detection certification limited liability company is precisely led in iron content analysis using Dongguan
Body Atomic Emission Spectrometer AES (ICP-OES) measurement.Fourier Transform Infrared Spectroscopy (FTIR) uses U.S. Thermo company
The measurement of 6700 type Fourier turn infrared instrument of Nicolet.Contact angle uses the OCA of Dataphysics company, Germany
The measurement of type contact angle measurement, test temperature are 25 DEG C.Scanning electron microscope (SEM), model JSM-6701F, Japan Electronics
Co., Ltd. (JEOL).
Cyclic voltammetry and constant current charge-discharge test, specific test condition are carried out using CHI 660E electrochemical workstation
Are as follows: use three-electrode system, 1.0M Na2SO4Make electrolyte, the foam nickel sheet positive electrode of CNT-COFc as working electrode,
Ag/AgCl (3.0M KCl) and Pt are respectively as reference and to electrode.
5, test result:
5.1, the structural analysis of CNT-COFc
" grafting rate " of ferrocene group can pass through thermogravimetric analysis (TG) in ferrocenyl carbon nanotube (CNT-COFc)
It is measured with inductively coupled plasma atomic emission spectrometer (ICP-OES).Carbon nanotube and ferrocenyl carbon nanotube
(CNT-COFc) as shown in Fig. 2, when carbon nanotube (CNT) is heated to 800 degree, residual mass accounts for just the TG figure in dry air
The 2.8wt% of prothyl amount, this residual substance are catalyst and impurity.And ferrocenyl carbon nanotube (CNT-COFc) is heated to
At 800 degree, residual mass accounts for the 6.4wt% of initial mass, it is assumed that and ferrocenyl is completely converted into iron oxide after air burning,
" grafting rate " for being computed ferrocenyl in CNT-COFc is 8.3wt%.Ferro element in CNT-COFc is measured by ICP-OES
Content is 1.8wt%, and the content for being converted to ferrocenyl is 6.0wt%, this is almost the same with TG test result.To sum up, two cyclopentadienyl
" grafting rate " of ferrocenyl is about 7.3wt% in iron-based carbon nanotube (CNT-COFc).
The wetability of sample CNT-COFc is characterized using water contact angle test, in general, if water contact angle is small
In 90 °, show that sample surfaces are hydrophily；Contact angle is smaller, and hydrophily is stronger.Water droplet is respectively at multi-walled carbon nanotube CNT (A)
As shown in figs.3 a and 3b with the upper viewgraph of cross-section of ferrocenyl carbon nanotube CNT-COFc (B).Carbon nanotube is by two cyclopentadienyls
After iron-based modification, surface hydrophilicity is significantly improved than unmodified sample, according to before the study found that the wetability of CNT is to electricity
Capacity is affected, and general hydrophily appropriate is conducive to specific capacitance.
Further the pattern of carbon nanotube CNT and ferrocenyl carbon nanotube CNT-COFc are characterized, carbon nanotube
The SEM of CNT and ferrocenyl carbon nanotube CNT-COFc scheme as illustrated in figures 4 a and 4b, it can be seen that after ferrocenyl modification,
CNT-COFc still maintains the pattern of CNT, i.e. the chemical modification whole rule degree that does not destroy CNT.
5.2, electro-chemical test
In order to study the chemical property for the ferrocenyl supercapacitor that CNT-COFc is constructed, cyclic voltammetric is carried out to it
Method (CV) and constant current charge-discharge test.Fig. 5 is CNT and CNT-COFc in 10mVs-1CV figure, it can be seen from the figure that CNT
CV figure with CNT-COFc is rectangle or class rectangle, and showing both materials all has good capacitance characteristic.It can also see
The CV curve of CNT-COFc has a pair of unconspicuous redox peaks between 0.0-0.4V out, this is probably derived from carbon to peak and receives
The CV of the contribution of the ferrocenyl of nanotube surface modification, original CNT schemes no redox peaks.From figure it has also been found that grafting ferrocene
After base, significantly increased in the area of same scan rate lower curve.Specific capacitance is calculated from the integral area of Fig. 5, calculation formula:Calculated result is as shown in Figure 6.As can be seen from Figure 6, in identical sweep speed 10mVs-1Under,
The specific capacitance 27.2Fg of original carbon nanotubes (CNT)-1, specific capacitance is 67.0Fg after being grafted ferrocenyl-1, that is, it is grafted two
After cyclopentadienyl is iron-based, specific capacitance is increased to 2.46 times, this may be derived from the ferrocenyl of good hydrophily and surface introducing after grafting.
Further CV figure of the research CNT-COFc under different scanning rates, as shown in fig. 7, as can be seen from the figure with sweep speed
From 10,20,50,100,200mVs-1Increase, the area of curve incrementally increases.Specific capacitance, meter are calculated from the integral area of Fig. 7
It is as shown in Figure 8 to calculate result.As can be seen from Figure 8 the specific capacitance of CNT-COFc declines with the increase of sweep speed.In 200mVs-1
When, specific capacitance 9.5Fg-1, specific capacitance conservation rate is 14.2%.
Charging and discharging curve of the CNT-COFc under different current densities is further studied by constant current charge-discharge test, such as
Shown in Fig. 9, curve shows good symmetry and linear character, embodies excellent super capacitor performance.Utilize formulaSpecific capacitance value of the CNT-COFc under different current densities is calculated from the discharge curve of Fig. 9, as shown in Figure 10,
Show that current density is followed successively by 0.4,0.8,1.2,1.6,2.0Ag-1When, specific capacitance is respectively 53.6,47.8,42.8,38.3,
34.1F·g-1.The above results show that CNT-COFc has superior super capacitor performance.Other than can be with fast charging and discharging,
Cycle life is also another key parameter of research.In 2.0Ag-1Lower progress CNT-COFc cycle life test, 5000
The result of secondary fast charging and discharging is as shown in figure 11, and specific capacitance value only decays 4% after finding 5000 circulations, shows that it has height
Service life.
In conclusion a kind of ferrocenyl supercapacitor provided by the invention.The present invention utilizes ferrocenyl carbon nanometer
Splendid redox characteristic and hydrophily are managed, can be used as the electrode material of supercapacitor, is made a kind of novel super
Grade capacitor, to greatly improve the chemical property of supercapacitor.Pass through the electrochemistry such as cyclic voltammetry, constant current charge-discharge
Characterization, find the supercapacitor current density be 0.2Ag-1When, specific capacitance 67.0Fg-1, it is unmodified carbon nanometer
2.46 times of pipe；In 2.0Ag-1The lower cycle life for carrying out CNT-COFc is tested, and specific capacitance value only decays after 5000 circulations
4%, show that CNT-COFc is a kind of good super capacitor anode material.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can
With improvement or transformation based on the above description, all these modifications and variations all should belong to the guarantor of appended claims of the present invention
Protect range.
Claims (8)
1. a kind of ferrocenyl supercapacitor, including working electrode, reference electrode and to electrode and electrolyte, feature exists
In the working electrode is prepared using ferrocenyl carbon nanotube, the chemical structural formula of the ferrocenyl carbon nanotube
It is as follows:
2. ferrocenyl supercapacitor according to claim 1, which is characterized in that the preparation method of the working electrode
Comprising steps of weighing ferrocenyl carbon nanotube, bonding agent and conductive agent are added, paste is tuned into, is pressed together on carrier, baking system
Obtain ferrocenyl carbon nanotube electrode.
3. ferrocenyl supercapacitor according to claim 2, which is characterized in that the preparation method of the working electrode
Specifically include step:
The ferrocenyl carbon nanotube for weighing 5mg, adds the bonding agent of 1mg and the conductive agent of 1mg, is tuned into paste, is pressed together on load
10h is toasted on body, at 100 DEG C, and ferrocenyl carbon nanotube electrode is made.
4. according to the described in any item ferrocenyl supercapacitors of claim 2-3, which is characterized in that the bonding agent is
60wt% polytetrafluoroethyl-ne aqueous solution.
5. according to the described in any item ferrocenyl supercapacitors of claim 2-3, which is characterized in that the conductive agent is second
Acetylene black.
6. according to the described in any item ferrocenyl supercapacitors of claim 2-3, which is characterized in that the carrier is foam
Nickel sheet.
7. ferrocenyl supercapacitor according to claim 6, which is characterized in that the size of the foam nickel sheet
For 1cm × 5cm.
8. ferrocenyl supercapacitor according to claim 1, which is characterized in that the reference electrode is Ag/AgCl,
Described is Pt to electrode, and the electrolyte is Na2SO4。
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103466595A (en) * | 2013-08-29 | 2013-12-25 | 福州大学 | Method for preparing ferrocene functionalized carbon nanotube composite material |
| CN104129776A (en) * | 2014-08-15 | 2014-11-05 | 北京万源工业有限公司 | Controllable preparation method of carboxyl functionalized carbon nanotube |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103466595A (en) * | 2013-08-29 | 2013-12-25 | 福州大学 | Method for preparing ferrocene functionalized carbon nanotube composite material |
| CN104129776A (en) * | 2014-08-15 | 2014-11-05 | 北京万源工业有限公司 | Controllable preparation method of carboxyl functionalized carbon nanotube |
Non-Patent Citations (2)
| Title |
|---|
| Covalent Grafting of Ferrocene to Vertically Aligned Carbon Nanofibers: Electron-transfer Processes at Nanostructured Electrodes;Elizabeth C. Landis等;《J. Phys. Chem. C》;20080924;第112卷;全文 |
| Noncovalent Modification of Carbon Nanotubes with Ferrocene-Amino Acid Conjugates for Electrochemical Sensing of Chemical Warfare Agent Mimics;Mohammad A. K. Khan等;《Analytical Chemistry》;20080401;第80卷(第7期);全文 |
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Application publication date: 20180202 Assignee: Guangzhou Aosheng Technology Co.,Ltd. Assignor: DONGGUAN University OF TECHNOLOGY Contract record no.: X2023990000096 Denomination of invention: A ferrocene-based supercapacitor Granted publication date: 20190402 License type: Common License Record date: 20230112 |