CN106971861B - The method for improving supercapacitor Schiff transition metal polymerization object electrode specific capacity - Google Patents
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Abstract
A method of supercapacitor Schiff transition metal polymerization object electrode specific capacity is improved, organic system supercapacitor field is belonged to.Two different conducting polymer electro-deposition are directly polymerize by the present invention on a current collector by two-step method.First under organic system by electro-deposition mode by Schiff transition metal polymerization object monomer electropolymerization in collector titanium sheet, dissolve aniline (AN) monomer under acid system later and aniline polymerization organized to the electrode material of conducting polymer Poly in pairs [M (Schiff)]/PANI supercapacitor by way of electropolymerization in the collector titanium sheet for having a kind of conducting polymer.Composite material exhibits go out exclusive pattern, which embodies more excellent capacitance characteristic when being used alone by the synergistic effect between two kinds of conducting polymers than any of them conducting polymer.The method of the present invention is simple, can be by this compound structure of the two and carbon material, further compound its performance as electrode material for super capacitor of raising such as transition metal oxide.
Description
Technical field
The present invention relates to one kind to improve supercapacitor Schiff transition metal polymerization object electrode in organic system
The method of specific capacity.The invention belongs to the electrode material of electrochemical energy storage, can be used for organic system supercapacitor field.
Background technique
21 century economic development is it in the weight of every country, and the energy is transported in a cornerstone of the state either national defence
With the guided missile of high and new technology, it is still used in low technology, appears in the electric cooker of diet daily life, all be unable to do without the energy.
It therefore is the height that must promote strategic position in national planning.Supercapacitor is provided simultaneously with physical capacitor and battery
Good characteristic can be discharged as General Physics capacitor higher as a kind of more novel energy storage energy source device
Discharge power, and powerful charge storage can typically be provided with as battery.
Supercapacitor as battery all mainly by component combinations such as collector, electrolyte, electrode material and diaphragms and
At the big bottleneck for limiting supercapacitor applications at present is that the specific capacity of electrode material.And conducting polymer is due to it
Excellent performance, material are easy to get, and the characteristics such as low in cost are widely used and electrode material for super capacitor.Schiff base mistake
Metal-containing polymer poly [M (Schiff)] is crossed to have a good application prospect as the new electrode materials of supercapacitor.With
Conventional conductive polymer is compared, and Schiff base transition metal polymerization object has apparent advantage, wherein wider potential change
Window and good chemical property make it be expected to reduce current supercapacitor and secondary cell in terms of storing energy density
Gap.In addition, Schiff base transition metal polymerization object preparation process is simple, cost is relatively low, is just meeting current super electricity
The development trend of field of containers.
Conducting polymer is usually by gripping the polymer of pi bond system institute after chemistry or electrochemical doping altogether with electronics
, doped conducting polymer has the electric conductivity of metalloid.Compared with metallic conductor, conducting polymer is in addition to close
It spends small, light weight, be easy outside the characteristics of molding, also there are some unique properties.American professor MacDiarmid is for the first time in acid
The research hotspot that conductive product polyaniline subsequently becomes conducting polymer field is obtained under the conditions of property.Relative to it
Its conducting polymer materials is easy to get with its raw material, synthesizes convenient, various structures and excellent physical property and good environment
Stability and the broad interest for causing researcher, become conducting polymer family and grind the hot spot to make internal disorder or usurp.And it is two different
The compound electrode material as supercapacitor of conducting polymer improves electrode material using synergistic effect between the two
The mode of specific capacity less mention.Electrochemical polymerization method prepares conducting polymer at the same time, passes through control electric current or control
Current potential makes polymerized monomer that oxidative polymerization occur on anode, forms conducting polymer and forms the high shape of specific surface area
Looks.Simultaneous electrochemical method synthesis conducting polymer has many advantages, such as that reaction condition is simple, easy to control, with high purity.
Summary of the invention
The purpose of the present invention is being provided in one kind in organic system by electropolymerization Polyaniline-modified supercapacitor use
Method of the Schiff transition metal polymerization object electrode to improve electrode material for super capacitor specific capacity.It is led using both
Synergistic effect between electric polymer significantly improves specific capacity of the Schiff base transition metal polymerization object as electrode material.For
Reach above-mentioned requirement, technical solution provided by the invention is carried out according to the following steps:
1, titanium sheet the processing of collector titanium sheet: is cut into the sheet that specification is 1cm × 3cm；It is put into the sodium carbonate of alkalinity
Water-bath is deoiled in solution is placed into the HCl of 30wt% with deionized water flushing, is washed with deionized water after impregnating 1.5~2.5h
Only；Clean titanium sheet one end (1cm × 1cm) is polished smooth with the sand paper of different model, until immaculate occurs.
2, polymerize Schiff transition metal polymerization object monomer: lower working electrode is afflux in organic three-electrode system
The work area of one end (1 × 1) in body titanium sheet, reference electrode Ag/AgCl, auxiliary electrode are the active carbon cloth of large area.It will
Schiff transition metal polymerization object monomer is dissolved in the low organic solvent of electron number in solution, and is added a certain amount of
Supporting electrolyte aggregates into electrode using electrochemical method.
3, polymerization aniline monomer constructs double conductive polymer electrodes materials: under inorganic acid system, utilizing three electrodes
System electropolymerization aniline monomer.Working electrode is the electrode that (2) step aggregates into, and reference electrode is mercury-mercurous sulfate electrode, auxiliary
Helping electrode is platinum electrode.Polymer fluid is that aniline monomer is dissolved in dilution heat of sulfuric acid.
Wherein, described in step 1, by the requirement of soda acid treated titanium sheet collector will meet collector, experiment is improved
Repeatability.
The type of Schiff transition metal polymerization object monomer described in step 2 include Me (Schiff) (Me=Ni, Co,
Mn, Pb, etc.), the concentration of monomer is between 1mmol/L-10mmol/L.The low organic solvent of electron number includes acetonitrile, benzene first
Supporting electrolyte includes tetrabutylammonium perchlorate (TBAP), Et simultaneously for nitrile, vinyl carbonate, propylene carbonate etc.4NBF4,
Et4NPF6(anion radius is followed successively by 0.241,0.333,0.435nm) (Me4N)BF4, (Et4N)BF4, (Bu4N)BF4(cation
Secondary is 0.47,0.56,0.96nm).
The concentration of aniline monomer described in step 3 is between 0.2mol/L-0.5mol/L.The concentration of sulfuric acid is in 0.5mol/
Between L-1.5mol/L.Polyaniline (PANI) polymerization includes constant flow method, constant-voltage method, cyclic voltammetry, impulse method.
Schiff transition metal polymerization object is electrodeposited into collector using the method for electrochemical polymerization by the method for the present invention
It is pure in organic system because of conducting polymer in titanium sheet that certain specific capacity is provided as electrode material in fake capacitance behavior.
The method of the present invention is on the basis of electropolymerization Schiff transition metal polymerization object in collector titanium sheet in acid body
System is lower to continue electropolymerization aniline, modifies Schiff transition metal conducting polymer.Double composite conductive polymers are placed on organic
Measured in system its specific capacity show its specific capacity than be used alone Schiff transition metal polymerization object electrode when promoted it is bright
It is aobvious.And preparation method can simply effectively improve its specific capacity.
Detailed description of the invention
Fig. 1 is the scanning electricity of supercapacitor Schiff transition metal polymerization object electrode material prepared by the present invention
Mirror (SEM) figure
Fig. 2 is the scanning electron microscope of supercapacitor conductive polymer polyanaline electrode material prepared by the present invention
(SEM) figure
Fig. 3 is the scanning electron microscope of supercapacitor Poly [M (Schiff)]/PANI electrode material prepared by the present invention
(SEM) figure
Fig. 4 is the cyclic voltammetric of supercapacitor Poly [M (Schiff)]/PANI electrode material prepared by the present invention
Curve
Fig. 5 is the constant current charge and discharge of supercapacitor Poly [M (Schiff)]/PANI electrode material prepared by the present invention
Electric curve
Fig. 6 is the different voltages of supercapacitor Poly [M (Schiff)]/PANI electrode material prepared by the present invention
The chrono-amperometric in step section is tested
Specific embodiment
It elaborates with reference to the accompanying drawings and examples to the present invention.Technical solution of the present invention is carried out clear, complete
Site preparation description, it is clear that the described embodiment is only a part of the embodiment of the present invention, instead of all the embodiments.Based on this
Embodiment in invention, every other reality obtained by those of ordinary skill in the art without making creative efforts
Example is applied, shall fall within the protection scope of the present invention.
Embodiment 1
Step 1: titanium sheet is cut into the sheet that specification is 1 × 3；Water-bath in the sodium carbonate liquor of alkalinity is put into go
The flushing of oil deionized water places into the HCl of 30wt%, is washed with deionized water after impregnating 2h；
Clean titanium sheet one end (1 × 1) is polished smooth with the sand paper of different model, until immaculate occurs.
Step 2: the electrolyte tetrabutylammonium perchlorate (TBAP) of 0.1mol/L, the Ni of 1mmol/L are dissolved in acetonitrile solution
(salphen), Ag/AgCl reference electrode is utilized under three-electrode system, large area active carbon cloth auxiliary electrode is as auxiliary electricity
Pole, using cyclic voltammetry electropolymerization Schiff transition metal polymerization object Ni (salphen), wherein scanning current potential is 0-1.3V
Scanning speed is 20mv/s, and scanning circle number 20 encloses.Chemical property after having polymerize under organic system is as shown in the figure.
Step 3: it is completed in three-electrode system inorganic using Polyaniline-modified Schiff transition metal polymerization object
Under acid system, working electrode is the electrode that second step aggregates into, and reference electrode is mercury-mercurous sulfate electrode, and auxiliary electrode is
Platinum electrode.Polymer fluid is that aniline monomer is dissolved in dilution heat of sulfuric acid, is later aggregated to aniline monomer using constant flow method
On Schiff transition metal polymerization object.It is 10min that wherein electric current, which is 0.5mA polymerization time,.
Embodiment 2
Step 1: titanium sheet is cut into the sheet that specification is 1 × 3；Water-bath in the sodium carbonate liquor of alkalinity is put into deoil use
Deionized water flushing places into the HCl of 30wt%, is washed with deionized water after impregnating 2h；By clean titanium sheet one end (1 × 1)
It is polished smooth with the sand paper of different model, until immaculate occurs.
Step 2: the electrolyte tetrabutylammonium perchlorate (TBAP) of 0.1mol/L, the Ni of 5mmol/L are dissolved in acetonitrile solution
(salphen), Ag/AgCl reference electrode is utilized under three-electrode system, large area active carbon cloth auxiliary electrode is as auxiliary electricity
Pole, using cyclic voltammetry electropolymerization Schiff transition metal polymerization object Ni (salphen), wherein scanning current potential is 0-1.3V
Scanning speed is 20mv/s, and scanning circle number 10 encloses.Chemical property after having polymerize under organic system is as shown in the figure.
Step 3: it is completed in three-electrode system inorganic using Polyaniline-modified Schiff transition metal polymerization object
Under acid system, working electrode is the electrode that second step aggregates into, and reference electrode is mercury-mercurous sulfate electrode, and auxiliary electrode is
Platinum electrode.Polymer fluid is that aniline monomer is dissolved in dilution heat of sulfuric acid, is later aggregated to aniline monomer using constant flow method
On Schiff transition metal polymerization object.It is 10min that wherein electric current, which is 0.5mA polymerization time,.
Embodiment 3
Step 1: titanium sheet is cut into the sheet that specification is 1 × 3；Water-bath in the sodium carbonate liquor of alkalinity is put into deoil use
Deionized water flushing places into the HCl of 30wt%, is washed with deionized water after impregnating 2h；By clean titanium sheet one end (1 × 1)
It is polished smooth with the sand paper of different model, until immaculate occurs.
Step 2: the electrolyte tetrabutylammonium perchlorate (TBAP) of 0.1mol/L, the Ni of 5mmol/L are dissolved in acetonitrile solution
(salphen), Ag/AgCl reference electrode is utilized under three-electrode system, large area active carbon cloth auxiliary electrode is as auxiliary electricity
Pole, using potentiostatic method electropolymerization Schiff transition metal polymerization object Ni (salphen), wherein polymerization current potential 0.85V polymerization
Time 20min.Chemical property after having polymerize under organic system is as shown in the figure.
Step 3: it is completed in three-electrode system inorganic using Polyaniline-modified Schiff transition metal polymerization object
Under acid system, working electrode is the electrode that second step aggregates into, and reference electrode is mercury-mercurous sulfate electrode, and auxiliary electrode is
Platinum electrode.Polymer fluid is that aniline monomer is dissolved in dilution heat of sulfuric acid, is later aggregated to aniline monomer using constant flow method
On Schiff transition metal polymerization object.It is 10min that wherein electric current, which is 0.5mA polymerization time,.
Embodiment 4
Step 1: titanium sheet is cut into the sheet that specification is 1 × 3；Water-bath in the sodium carbonate liquor of alkalinity is put into deoil use
Deionized water flushing places into the HCl of 30wt%, is washed with deionized water after impregnating 2h；By clean titanium sheet one end (1 × 1)
It is polished smooth with the sand paper of different model, until immaculate occurs.
Step 2: the electrolyte tetrabutylammonium perchlorate (TBAP) of 0.1mol/L, the Ni of 5mmol/L are dissolved in acetonitrile solution
(salphen), Ag/AgCl reference electrode is utilized under three-electrode system, large area active carbon cloth auxiliary electrode is as auxiliary electricity
Pole, using potentiostatic method electropolymerization Schiff transition metal polymerization object Ni (salphen), wherein polymerization current potential 0.85V polymerization
Time 20min.Chemical property after having polymerize under organic system is as shown in the figure.
Step 3: it is completed in three-electrode system inorganic using Polyaniline-modified Schiff transition metal polymerization object
Under acid system, working electrode is the electrode that second step aggregates into, and reference electrode is mercury-mercurous sulfate electrode, and auxiliary electrode is
Platinum electrode.Polymer fluid is that aniline monomer is dissolved in dilution heat of sulfuric acid, is later aggregated to aniline monomer using cyclic voltammetry
On Schiff transition metal polymerization object.Wherein polymerization potential range is that -0.4V-0.6V polymerization circle number 5 encloses.Scanning speed is
20mv/s。
The above embodiments are merely illustrative of the technical solutions of the present invention rather than is limited, the common skill of fields
Art personnel should be appreciated that referring to above-described embodiment can with modifications or equivalent substitutions are made to specific embodiments of the invention,
These are applying for pending claim protection model without departing from any modification of spirit and scope of the invention or equivalent replacement
Within enclosing.
Claims (8)
1. a kind of method for improving supercapacitor Schiff transition metal polymerization object electrode specific capacity, which is characterized in that
The following steps are included:
(1) titanium sheet the processing of collector titanium sheet: is cut into the sheet that specification is 1cm × 3cm；It is put into the sodium carbonate liquor of alkalinity
Middle water-bath is deoiled to be placed into the HCl of 30wt% with deionized water flushing, is washed with deionized water after impregnating 1.5~2.5h；It will
The sand paper of clean titanium sheet one end different model polishes smooth, until immaculate occurs；
(2) polymerize Schiff transition metal polymerization object monomer: under in organic three-electrode system, working electrode is collector
The work area of one end in titanium sheet, reference electrode Ag/AgCl, auxiliary electrode are the active carbon cloth of large area；By Schiff
Transition metal polymerization object monomer is dissolved in the low organic solvent of electron number, and adds a certain amount of supporting electrolyte, benefit
Electrochemically aggregate into electrode；
(3) polymerization aniline monomer constructs double conductive polymer electrodes materials: under inorganic acid system, utilizing three-electrode system
Electropolymerization aniline monomer；Working electrode is the electrode that (2) step aggregates into, and reference electrode is mercury-mercurous sulfate electrode, auxiliary electricity
Extremely platinum electrode；Polymer fluid is that aniline monomer is dissolved in dilution heat of sulfuric acid.
2. a kind of raising supercapacitor according to claim 1 Schiff transition metal polymerization object electrode specific capacity
Method, which is characterized in that in step (1), by soda acid handle certain specification titanium sheet so that it is met the requirement of collector, mention
The repeatability of height experiment.
3. a kind of raising supercapacitor according to claim 1 Schiff transition metal polymerization object electrode specific capacity
Method, which is characterized in that in step (2), the type of Schiff transition metal polymerization object monomer includes Me (Schiff),
Middle Me=Ni, Co, Mn, Pb, the concentration of monomer is between 1mmol/L-10mmol/L.
4. a kind of raising supercapacitor according to claim 1 Schiff transition metal polymerization object electrode specific capacity
Method, which is characterized in that in step (2), the low organic solvent of electron number includes acetonitrile, benzonitrile, vinyl carbonate, third
Olefinic carbon acid esters.
5. a kind of raising supercapacitor according to claim 1 Schiff transition metal polymerization object electrode specific capacity
Method, which is characterized in that in step (2), supporting electrolyte includes TBAP, Et4NBF4, Et4NPF6, (Me4N)BF4, (Et4N)
BF4, (Bu4N)BF4, wherein the anion radius of TBAP is 0.241nm, Et4NBF4Anion radius be 0.333nm,
Et4NPF6Anion radius be 0.435nm, (Me4N)BF4Cation radius be 0.47nm, (Et4N)BF4Cation half
Diameter is 0.56nm, (Bu4N) cation radius of BF is 0.96nm.
6. a kind of raising supercapacitor according to claim 1 Schiff transition metal polymerization object electrode specific capacity
Method, which is characterized in that in step (2), the method for electrochemical polymerization includes cyclic voltammetry, potentiostatic method, impulse method.
7. a kind of raising supercapacitor according to claim 1 Schiff transition metal polymerization object electrode specific capacity
Method, which is characterized in that in step (3), the concentration of aniline monomer is between 0.2mol/L-0.5mol/L, the concentration of sulfuric acid
Between 0.5mol/L-1.5mol/L.
8. a kind of raising supercapacitor according to claim 1 Schiff transition metal polymerization object electrode specific capacity
Method, which is characterized in that in step (3), polyaniline (PANI) polymerization include constant flow method, constant-voltage method, cyclic voltammetry,
Impulse method.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1083259A (en) * | 1992-07-23 | 1994-03-02 | 松下电器产业株式会社 | A kind of ion conducting polymer electrolyte |
| US20070065719A1 (en) * | 2003-10-14 | 2007-03-22 | Alexander Timonov | Electrode for energy storage devices and electrochemical supercapacitor based on said electrode |
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2017
- 2017-05-09 CN CN201710321499.XA patent/CN106971861B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1083259A (en) * | 1992-07-23 | 1994-03-02 | 松下电器产业株式会社 | A kind of ion conducting polymer electrolyte |
| US20070065719A1 (en) * | 2003-10-14 | 2007-03-22 | Alexander Timonov | Electrode for energy storage devices and electrochemical supercapacitor based on said electrode |
Non-Patent Citations (3)
| Title |
|---|
| "Electropolymerization and electrochemical behavior of nickel Schiff base complexes with different groups between imine linkages";Cheng Chen, Xinping Li, Fuhai Deng and Jianling Li;《RSC Advances》;20160810;第6卷(第83期);第79894-79899页 * |
| "Electropolymerization of Ni(salen) on carbon nanotube carrier as a capacitive material by pulse potentiostatic method";LI JianLing, GAO Fei, ZHANG YaKun, KANG FeiYu,et al.;《Science China-Chemistry》;20120607;第55卷(第7期);第1338-1344页 * |
| "Growth and Electrochemical Behavior of Poly[Ni(saldMp)] on Carbon Nanotubes as Potential Supercapacitor Materials";Yakun Zhang, Jianling Li, Feiyu Kang, Xindong Wang,et al.;《Bulletin of the Korean Chemical Society》;20120620;第33卷(第6期);第1972-1978页 * |
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