CN106783221A - A kind of organic/inorganic hybrid supercapacitor electrode material and preparation method thereof - Google Patents
A kind of organic/inorganic hybrid supercapacitor electrode material and preparation method thereof Download PDFInfo
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- CN106783221A CN106783221A CN201611027936.9A CN201611027936A CN106783221A CN 106783221 A CN106783221 A CN 106783221A CN 201611027936 A CN201611027936 A CN 201611027936A CN 106783221 A CN106783221 A CN 106783221A
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- electrode material
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- silsesquioxane
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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
- H01G11/48—Conductive polymers
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- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01G11/24—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
-
- 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
-
- 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
A kind of preparation method of organic/inorganic hybrid supercapacitor electrode material, step is as follows：Silsesquioxane alkanes compound is dispersed in acidic aqueous solution, is disperseed under the hybrid mode of mechanical agitation and ultrasonic wave.The presoma of conductive polymer subclass compound is added, in mechanical agitation and ultrasonic wave and with continuing to be uniformly dispersed under mode.By disperse oxidant after acidic aqueous solution, refrigeration, it is added dropwise in the presoma and silsesquioxane mixed solution of conductive polymer subclass compound, continues to disperse under the hybrid mode of mechanical agitation and ultrasonic wave.After reaction terminates, mixed liquor is washed till filtrate with water and absolute ethyl alcohol successively colourless, organic/inorganic hybrid supercapacitor electrode material is obtained after vacuum drying.The organic/inorganic hybrid supercapacitor electrode material that the present invention is obtained has the advantages that with low cost, process is simple, compound with regular structure, electric conductivity is good, good cycling stability, excellent heat stability, with good prospects for commercial application.
Description
Technical field
It is compound super the present invention relates to the preparation field of the electrode material of ultracapacitor, more particularly to a kind of organic/inorganic
Level capacitor electrode material and preparation method thereof.
Background technology
Into after 21 century, traditional fossil energy cannot have been met needed for population increases, the existence of the mankind and society
Sustainable development because energy problem will be faced with huge challenge.Therefore, find and develop the task of sustainable energy
It is extremely urgent.At present, sustainable energy is including solar energy, wind energy, tide energy and geothermal energy etc., but these energy conversions are electricity
Can all there are problems that fluctuation and intermittent, ultracapacitor as a kind of new energy storage device, in the development of new energy
In show powerful application prospect.
Electrode material is the core part of ultracapacitor, the features such as need to possess high specific energy, long circulation life and high power.
Common electrodes material can be divided into：Carbon material, transition metal oxide and conducting polymer.Conducting polymer, such as polyaniline, poly- pyrrole
The features such as coughing up with polythiophene etc. because synthesizing easy, cheap and environment-friendly, causes extensive concern.But conducting polymer is made
It is electrode material, mainly there is that cycle life is short and the low shortcoming of energy density, and limits it and realize industrial applications.In order to
The cycle life and energy density of conducting polymer are improved, nano-particle can be often incorporated into conducting polymer, form compound
Electrode material.Because nano-particle has big specific surface area, the contact area of electrode material and electrolyte can be improved, be conducive to from
The insertion and abjection of son, improve the efficiency of discharge and recharge.Silsesquioxane alkanes compound is a kind of organic/inorganic hybridization material, collection
Organic and inorganic materials excellent properties are in one.It is combined with conducting polymer, chemical property is can obtain excellent and thermally-stabilised
The good combination electrode material of property.
The content of the invention
Goal of the invention：The method that this patent is related to is a kind of organic/inorganic hybrid supercapacitor electrode material and its system
Preparation Method.Organic/inorganic hybrid supercapacitor electrode material is conductive polymer subclass compound and silsesquioxane alkanes chemical combination
The complex of thing；The pattern of combination electrode material is nanofiber hierarchical structure of the surface with nano-particle, nano-particle
Particle diameter is 1~3nm, and the length of nanofiber is 300~800nm, a diameter of 50~80nm of nanofiber.
Technical scheme：To achieve these goals, the present invention relates to a kind of organic/inorganic hybrid supercapacitor electrode material
Material and preparation method thereof, the method comprises the following steps：
(1) silsesquioxane alkanes compound is dispersed in the acidic aqueous solution of 0.05~2mol/L, in mechanical agitation and
The hybrid mode of ultrasonic wave disperses 0.5~2h, and the concentration of silsesquioxane alkanes compound is 0.01~1wt%；
(2) to the presoma that conductive polymer subclass compound is added in the mixed solution of step (1), in mechanical agitation and super
The hybrid mode of sound wave disperses 0.5~2h, is subsequently placed in ice-water bath, and keeping temperature is 0~4 DEG C, refrigerates 0.5~2h,
The precursor concentration of conductive polymer subclass compound is 0.05~0.5mol/L；
(3) by disperse oxidant in the acidic aqueous solution of 0.05~2mol/L, 0.5~2h, oxidation are refrigerated at 0~4 DEG C
The concentration of agent is 0.05~0.5mol/L；
(4) under conditions of mechanical agitation and ultrasonic wave and use, the mixed solution of step (3) is added dropwise to step
(2) in mixed solution, keeping temperature is 0~4 DEG C, and the reaction time is 0.5~2h；
(5) after the reaction of step (4) terminates, mixed liquor is washed till filtrate with water and absolute ethyl alcohol successively colourless, vacuum
Organic/inorganic hybrid supercapacitor electrode material is obtained after drying.
Acidic aqueous solution described in step (1) and (3) is the water-soluble of hydrochloric acid, sulfuric acid, perchloric acid or dodecyl sodium sulfonate
Liquid.
Silsesquioxane alkanes compound described in step (1) is aminosilsesquioxane, carboxyl silsesquioxane, sulfonic acid
Base silsesquioxane.
Conductive polymer subclass compound described in step (2) is polyaniline, polythiophene and polypyrrole and its derivative.
Mechanical agitation rotating speed described in step (1), (2) and (4) is 200~400rpm, ultrasonic frequency is 30~
50kHz。
Oxidant described in step (3) is ammonium persulfate, potassium peroxydisulfate and hydrogen peroxide.
The advantage of the invention is that：The organic/inorganic hybrid supercapacitor electrode material that the present invention is obtained has cost
Cheap, process is simple, compound with regular structure, electric conductivity are good, good cycling stability, excellent heat stability the advantages of, with good
Prospects for commercial application.
Brief description of the drawings
Fig. 1 is 1 polyaniline of embodiment/amido silsesquioxane (PANI/POSS-NH2) combination electrode material Electronic Speculum shine
Piece.
Fig. 2 is 1 polyaniline of embodiment/amido silsesquioxane (PANI/POSS-NH2) combination electrode material and pure polyphenyl
In the cyclic voltammetry curve of 100mV/s sweep speeds, wherein abscissa is current potential to amine (PANI) electrode material, and ordinate is electricity
Stream.
Specific embodiment
Embodiment 1：
(1) amido silsesquioxane is dispersed in the aqueous hydrochloric acid solution of 50mL 1mol/L, its concentration is 0.02wt%,
Ultrasonic disperse 0.5h, supersonic frequency is 40kHz；
(2) aniline is added in the hydrochloric acid solution of above-mentioned amido silsesquioxane, monomer concentration is 0.5mol/L, and machinery is stirred
Lower dispersion 0.5h by the way of ultrasonic wave is mixed and stirred, mixing speed is 300rpm, and supersonic frequency is 40kHz；
(3) ammonium persulfate is dispersed in the aqueous hydrochloric acid solution of 50mL 1mol/L, 0.5h is refrigerated at 0 DEG C, its concentration is
0.5mol/L；
(4) mixed solution of aniline is placed in ice-water bath, keeping temperature is 0 DEG C of 0.5h, and low whipping speed is 300rpm
Mechanical agitation and supersonic frequency be by the way of 40kHz ultrasonic waves under, the mixed solution of the ammonium persulfate after dropwise refrigerating is protected
Temperature is held for 0 DEG C；
(5) after ammonium persulfate mixed solution completion of dropping, low whipping speed is that 300rpm mechanical agitations and supersonic frequency are
Under by the way of 40kHz ultrasonic waves, the reaction time is 1h.After reaction terminates, mixed liquor is washed with water and absolute ethyl alcohol successively
Colourless to filtrate, after vacuum drying 24h, temperature is 40 DEG C.Obtain polyaniline/amido silsesquioxane combination electrode material.
Embodiment 2：
(1) amido silsesquioxane is dispersed in the aqueous hydrochloric acid solution of 50mL 1mol/L, its concentration is 0.04wt%,
Ultrasonic disperse 0.5h, supersonic frequency is 40kHz；
(2) aniline is added in the hydrochloric acid solution of above-mentioned amido silsesquioxane, monomer concentration is 0.5mol/L, and machinery is stirred
Lower dispersion 0.5h by the way of ultrasonic wave is mixed and stirred, mixing speed is 300rpm, and supersonic frequency is 40kHz；
(3) ammonium persulfate is dispersed in the aqueous hydrochloric acid solution of 50mL 1mol/L, 0.5h is refrigerated at 0 DEG C, its concentration is
0.5mol/L；
(4) mixed solution of aniline is placed in ice-water bath, keeping temperature is 0 DEG C of 0.5h, and low whipping speed is 300rpm
Mechanical agitation and supersonic frequency be by the way of 40kHz ultrasonic waves under, the mixed solution of the ammonium persulfate after dropwise refrigerating is protected
Temperature is held for 0 DEG C；
(5) after ammonium persulfate mixed solution completion of dropping, low whipping speed is that 300rpm mechanical agitations and supersonic frequency are
Under by the way of 40kHz ultrasonic waves, the reaction time is 1h.After reaction terminates, mixed liquor is washed with water and absolute ethyl alcohol successively
Colourless to filtrate, after vacuum drying 24h, temperature is 40 DEG C.Obtain polyaniline/amido silsesquioxane combination electrode material.
Embodiment 3：
(1) amido silsesquioxane is dispersed in the aqueous hydrochloric acid solution of 50mL 1mol/L, its concentration is 0.06wt%,
Ultrasonic disperse 0.5h, supersonic frequency is 40kHz；
(2) aniline is added in the hydrochloric acid solution of above-mentioned amido silsesquioxane, monomer concentration is 0.5mol/L, and machinery is stirred
Lower dispersion 0.5h by the way of ultrasonic wave is mixed and stirred, mixing speed is 300rpm, and supersonic frequency is 40kHz；
(3) ammonium persulfate is dispersed in the aqueous hydrochloric acid solution of 50mL 1mol/L, 0.5h is refrigerated at 0 DEG C, its concentration is
0.5mol/L；
(4) mixed solution of aniline is placed in ice-water bath, keeping temperature is 0 DEG C of 0.5h, and low whipping speed is 300rpm
Mechanical agitation and supersonic frequency be by the way of 40kHz ultrasonic waves under, the mixed solution of the ammonium persulfate after dropwise refrigerating is protected
Temperature is held for 0 DEG C；
(5) after ammonium persulfate mixed solution completion of dropping, low whipping speed is that 300rpm mechanical agitations and supersonic frequency are
Under by the way of 40kHz ultrasonic waves, the reaction time is 1h.After reaction terminates, mixed liquor is washed with water and absolute ethyl alcohol successively
Colourless to filtrate, after vacuum drying 24h, temperature is 40 DEG C.Obtain polyaniline/amido silsesquioxane combination electrode material.
Intersection example of the invention is the foregoing is only, is not intended to limit the invention, to those skilled in the art
For can obviously do many improvement, all any modifications within the spirit and principles in the present invention, made, replace on an equal basis
Change, improve, should be included within the scope of protection of the invention.
Claims (7)
1. a kind of organic/inorganic hybrid supercapacitor electrode material, it is characterised in that：Organic/inorganic hybrid supercapacitor
Electrode material is the complex of conductive polymer subclass compound and silsesquioxane alkanes compound；The pattern of combination electrode material is
Nanofiber hierarchical structure of the surface with nano-particle, the particle diameter of nano-particle is 1~3nm, and the length of nanofiber is 300
~800nm, a diameter of 50~80nm of nanofiber.
2. one kind prepares a kind of organic/inorganic hybrid supercapacitor electrode material as claimed in claim 1, it is characterized in that, bag
Include following steps：
(1) silsesquioxane alkanes compound is dispersed in the acidic aqueous solution of 0.05~2mol/L, in mechanical agitation and ultrasound
The hybrid mode of ripple disperses 0.5~2h, and the concentration of silsesquioxane alkanes compound is 0.01~1wt%；
(2) to the presoma that conductive polymer subclass compound is added in the mixed solution of step (1), in mechanical agitation and ultrasonic wave
Hybrid mode disperse 0.5~2h, be subsequently placed in ice-water bath, keeping temperature is 0~4 DEG C, refrigerates 0.5~2h, conductive
The precursor concentration of macromolecule compound is 0.05~0.5mol/L；
(3) by disperse oxidant in the acidic aqueous solution of 0.05~2mol/L, 0.5~2h is refrigerated at 0~4 DEG C, oxidant
Concentration is 0.05~0.5mol/L；
(4) under conditions of mechanical agitation and ultrasonic wave and use, the mixed solution of step (3) is added dropwise to step (2)
In mixed solution, keeping temperature is 0~4 DEG C, and the reaction time is 0.5~2h；
(5) after the reaction of step (4) terminates, mixed liquor is washed till filtrate with water and absolute ethyl alcohol successively colourless, vacuum drying
After obtain organic/inorganic hybrid supercapacitor electrode material.
3. preparation method according to claim 2, it is characterised in that：Acidic aqueous solution described in step (1) and (3) is
The aqueous solution of hydrochloric acid, sulfuric acid, perchloric acid or dodecyl sodium sulfonate.
4. preparation method according to claim 2, it is characterised in that：Silsesquioxane alkanes chemical combination described in step (1)
Thing is aminosilsesquioxane, carboxyl silsesquioxane, sulfonic group silsesquioxane.
5. preparation method according to claim 2, it is characterised in that：Conductive polymer subclass chemical combination described in step (2)
Thing is polyaniline, polythiophene and polypyrrole and its derivative.
6. preparation method according to claim 2, it is characterised in that：Mechanical agitation described in step (1), (2) and (4)
Rotating speed is 200~400rpm, and ultrasonic frequency is 30~50kHz.
7. preparation method according to claim 2, it is characterised in that：Oxidant described in step (3) is ammonium persulfate,
Potassium peroxydisulfate and hydrogen peroxide.
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| CN201611027936.9A CN106783221A (en) | 2016-11-18 | 2016-11-18 | A kind of organic/inorganic hybrid supercapacitor electrode material and preparation method thereof |
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| CN201611027936.9A CN106783221A (en) | 2016-11-18 | 2016-11-18 | A kind of organic/inorganic hybrid supercapacitor electrode material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108538612A (en) * | 2018-03-30 | 2018-09-14 | 徐州工业职业技术学院 | A kind of preparation method of the N doping carbon/manganese dioxide composite electrode material of porous intercommunication network |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010594A (en) * | 2010-10-26 | 2011-04-13 | 东华大学 | Method for preparing conductive polymer/silsesquioxane composite electrode material |
| CN104201007A (en) * | 2014-08-29 | 2014-12-10 | 中科院广州化学有限公司 | Carbon nanomaterial-based flexible super capacitor electrode material and preparation method for same |
-
2016
- 2016-11-18 CN CN201611027936.9A patent/CN106783221A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010594A (en) * | 2010-10-26 | 2011-04-13 | 东华大学 | Method for preparing conductive polymer/silsesquioxane composite electrode material |
| CN104201007A (en) * | 2014-08-29 | 2014-12-10 | 中科院广州化学有限公司 | Carbon nanomaterial-based flexible super capacitor electrode material and preparation method for same |
Non-Patent Citations (4)
| Title |
|---|
| SHANXIN XIONG等: ""Enhancement of Electrochromic Contrast by Tethering Conjugated Polymer Chains onto Polyhedral Oligomeric Silsesquioxane Nanocages"", 《MACROMOLECULAR RAPID COMMUNICATIONS》 * |
| WEIHONG LIN等: ""Hierarchical porous polyaniline–silsesquioxane conjugated hybrids with enhanced electrochemical capacitance"", 《RSC ADVANCES》 * |
| 李英芝: ""聚苯胺基纳米复合材料的制备及在超级电容器中的应用"", 《中国博士学位论文全文数据库 工程科技Ⅱ辑》 * |
| 荣耀 等: ""笼型八聚倍半硅氧烷与聚苯胺复合物的合成与表征"", 《应用化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108538612A (en) * | 2018-03-30 | 2018-09-14 | 徐州工业职业技术学院 | A kind of preparation method of the N doping carbon/manganese dioxide composite electrode material of porous intercommunication network |
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Application publication date: 20170531 |