CN108364794A - A kind of preparation method based on carbon cloth growth in situ tungstic acid electrode material for super capacitor - Google Patents
A kind of preparation method based on carbon cloth growth in situ tungstic acid electrode material for super capacitor Download PDFInfo
- Publication number
- CN108364794A CN108364794A CN201810044071.XA CN201810044071A CN108364794A CN 108364794 A CN108364794 A CN 108364794A CN 201810044071 A CN201810044071 A CN 201810044071A CN 108364794 A CN108364794 A CN 108364794A
- Authority
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- China
- Prior art keywords
- carbon cloth
- tungstic acid
- preparation
- acid
- electrode material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 31
- 239000004744 fabric Substances 0.000 title claims abstract description 31
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 title claims abstract description 15
- 239000003990 capacitor Substances 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000007772 electrode material Substances 0.000 title claims abstract description 8
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- YOUIDGQAIILFBW-UHFFFAOYSA-J tetrachlorotungsten Chemical compound Cl[W](Cl)(Cl)Cl YOUIDGQAIILFBW-UHFFFAOYSA-J 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract 2
- -1 by treated Chemical compound 0.000 abstract 1
- 239000008151 electrolyte solution Substances 0.000 abstract 1
- 238000007654 immersion Methods 0.000 abstract 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 16
- 239000000463 material Substances 0.000 description 11
- 235000019441 ethanol Nutrition 0.000 description 8
- 229960002163 hydrogen peroxide Drugs 0.000 description 8
- 150000007513 acids Chemical class 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
Classifications
-
- 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES 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
-
- 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
The invention discloses a kind of preparation methods based on carbon cloth growth in situ tungstic acid electrode material for super capacitor.Main preparation process is as follows：Carbon cloth is immersed in and carries out hydrophilic treated a whole night in hydrochloric acid, by treated, carbon cloth is immersed in the seed solution of wolframic acid, it is sintered in Muffle furnace to obtain the carbon cloth containing tungstic acid seed after the completion of immersion, then obtained carbon cloth is put into progress hydro-thermal reaction in the ethanol solution containing tungsten chloride and obtains a kind of electrode material that capacitive property is excellent, specific capacity is 5mA cm in current density‑2Shi Keda 600mF cm‑2, the ultracapacitor prepared in this approach is with good capacitive property.Present existing work is difficult effectively to promote the super electrical property of tungstic acid to be primarily due to the electric conductivity of tungstic acid difference and react in the electrolytic solution insufficient.Therefore, improve tungstic acid electric conductivity increased its reaction active site be vital.The present invention is effectively increased active site and electric conductivity to improve super electrical property by growing into tungstic trioxide nano-slice on the extremely strong carbon cloth of electric conductivity.
Description
Technical field
The invention belongs to energy-storage battery fields, and in particular to a kind of preparation side of the tungsten trioxide material with porous structure
Method.
Background technology
Ultracapacitor is since fast with charging rate, stable circulation performance is good, good temp characteristic, energy saving and environmentally friendly etc. special
Point can do the substitute of traditional chemical battery to a certain extent, the traction power source of vehicle and startup power supply etc. all
It is with a wide range of applications.The popularization of ultracapacitor, it will help the consumption of the chemical fuels such as oil, mitigate to oil into
Mouthful dependence, contribute to national oil safe, and help to solve city automobile tail gas pollution, lead-acid battery pollution etc. to ask
Topic.
Tungstic acid is the basic material for doing electrode of super capacitor, and tungstic acid is n-type semiconductor, nontoxic, tool
There are good physicochemical properties, and this material price is cheap with very high theoretical specific capacity and stable well
Property.But tungstic acid electric conductivity is poor, and present work is difficult that effectively improve its super electrical property may be because can
Participate in the deficiency of the active site of reaction.This tungsten trioxide material that the present invention selects has after hydro-thermal process by piece group
At flower-like structure.The active site for not only helping increase reaction, also has good conductive property, so this three oxidation
Tungsten material is a kind of electrode material for super capacitor of better performances.
Invention content
It is an object of the invention to develop a kind of electrode material for super capacitor of better performances, develop a kind of environmentally friendly without dirt
Dye and high performance electrode material for super capacitor.The technical solution adopted in the present invention is：Tungstic acid is this cheap steady
Fixed material carries out hydro-thermal preparation and is allowed to grow on carbon cloth, and quick and easy prepares porous carbon materials.
1) a certain size carbon cloth is dipped to stand in concentrated hydrochloric acid and carries out hydrophilic treated.
2) carbon cloth that step 1 obtains is cleaned with deionized water, is dried；
3) carbon cloth that step 2 obtains is immersed in the hydrogenperoxide steam generator of wolframic acid makes wolframic acid be attached on carbon cloth；
4) it is put by the carbon cloth of taking-up step 3 is thermally treated resulting in the carbon containing tungstic acid seed in Muffle furnace
Cloth；
5) carbon cloth that step 4 obtains is put into the ethanol solution of tungsten chloride and carries out 7h respectively, the hydro-thermal reaction of 8h and 9h；
6) obtained carbon cloth is cut into the size of 1cm*1cm；
7) electrode slice made is packaged test by electricity container device.
Step 1 soaking time is 12h.
3.1g wolframic acids are dissolved in 50mL hydrogen peroxide by step 3.
Step 4 heat treatment temperature is 500 DEG C of two hours of heat preservation.
Tungsten chloride is 0.6g in step 5, is dissolved in 70mL ethyl alcohol, and performance is best when wherein the hydro-thermal time is 8h.
Compared with existing super capacitor material, it is an advantage of the invention that being grown in flexibility using the material of cheap stabilization
Capacitor can be made to flexible device in substrate and facilitate wearing, this can become later trend.Tungstic acid is made flower-shaped
Structure does super capacitor material, and this material has the specific surface area of superelevation, has good super electrical property.This material
Ultracapacitor is 5mA cm in current density because of its high-specific surface area, specific capacity-2Shi Nengda 600mF cm-2。
Description of the drawings
Fig. 1 is SEM and the TEM figure for the tungstic trioxide nano-slice with porous structure that specific embodiment 1 obtains, hence it is evident that can
See with apparent sheet and porous structure；
Fig. 2 is the performance of the supercapacitor that specific embodiment 1 obtains the tungstic trioxide nano-slice with porous structure, gained
Tungstic trioxide nano-slice can be in 5mA cm-2Current density under reach 600mF cm-2Super electrical property.
Specific implementation mode
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
Attached drawing, the technical solution of the embodiment of the present invention is clearly and completely described.Obviously, described embodiment is this hair
Bright a part of the embodiment, instead of all the embodiments.Based on described the embodiment of the present invention, ordinary skill
The every other embodiment that personnel are obtained under the premise of without creative work, shall fall within the protection scope of the present invention.
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
1) carbon cloth 12 hours in concentrated hydrochloric acid are immersed in then take out and cleaned up with deionized water；
2) 3.13g wolframic acids are weighed to be dissolved in 50mL hydrogen peroxide.The carbon cloth handled well is immersed in above-mentioned wolframic acid
In hydrogenperoxide steam generator；
3) drying is put into the heat treatment that 500 DEG C of two hours are carried out in Muffle furnace after taking out；
4) 0.6g tungsten chlorides are weighed to be dissolved in 70mL ethyl alcohol, the carbon cloth being heat-treated are put into above-mentioned ethanol solution, so
It is sealed to the reaction for carrying out 8 hours in reaction kettle in 100 DEG C of baking ovens afterwards.
Embodiment 2
1) carbon cloth 12 hours in concentrated hydrochloric acid are immersed in then take out and cleaned up with deionized water；
2) 3.13g wolframic acids are weighed to be dissolved in 50mL hydrogen peroxide.The carbon cloth handled well is immersed in above-mentioned wolframic acid
In hydrogenperoxide steam generator；
3) drying is put into the heat treatment that 500 DEG C of two hours are carried out in Muffle furnace after taking out；
4) 0.6g tungsten chlorides are weighed to be dissolved in 70mL ethyl alcohol, the carbon cloth being heat-treated are put into above-mentioned ethanol solution, so
It is sealed to the reaction for carrying out 7 hours in reaction kettle in 100 DEG C of baking ovens afterwards.
Embodiment 3
1) carbon cloth 12 hours in concentrated hydrochloric acid are immersed in then take out and cleaned up with deionized water；
2) 3.13g wolframic acids are weighed to be dissolved in 50mL hydrogen peroxide.The carbon cloth handled well is immersed in above-mentioned wolframic acid
In hydrogenperoxide steam generator；
3) drying is put into the heat treatment that 500 DEG C of two hours are carried out in Muffle furnace after taking out；
4) 0.6g tungsten chlorides are weighed to be dissolved in 70mL ethyl alcohol, the carbon cloth being heat-treated are put into above-mentioned ethanol solution, so
It is sealed to the reaction for carrying out 9 hours in reaction kettle in 100 DEG C of baking ovens afterwards.
It should be understood that although with reference to its illustrative embodiment, particularly shown and description is carried out to the present invention,
It should be understood by those skilled in the art that without departing substantially from the spirit and model by the present invention as defined in the claims
Under conditions of enclosing, the variation of various forms and details can be carried out wherein, can carry out the arbitrary combination of various embodiments.
Claims (5)
1. a kind of preparation method based on carbon cloth growth in situ tungstic acid electrode material for super capacitor, it is characterised in that described
Method includes the following steps：
1) carbon cloth is immersed in and carries out hydrophilic treated a whole night in hydrochloric acid；
2) by treated, carbon cloth is immersed in the seed solution of wolframic acid；
3) it is sintered to obtain the carbon cloth containing tungstic acid seed in Muffle furnace after the completion of impregnating；
4) obtained carbon cloth is put into the ethanol solution containing tungsten chloride and carries out hydro-thermal reaction；
5) chemical property of above-mentioned product is tested with electrochemical workstation.
2. preparation method according to claim 1, which is characterized in that concentration of hydrochloric acid described in step 1) is 12M.
3. preparation method according to claim 1, which is characterized in that seed solution described in step 2) disperses for wolframic acid
Liquid, soaking time 10 minutes.
4. preparation method according to claim 1, which is characterized in that the heat treatment process described in step 3) is air
In calcine 2 hours at 500 DEG C.
5. preparation method according to claim 1, which is characterized in that described in step 4), hydrothermal process is at 100 DEG C
Lower reaction 8 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810044071.XA CN108364794A (en) | 2018-01-10 | 2018-01-10 | A kind of preparation method based on carbon cloth growth in situ tungstic acid electrode material for super capacitor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810044071.XA CN108364794A (en) | 2018-01-10 | 2018-01-10 | A kind of preparation method based on carbon cloth growth in situ tungstic acid electrode material for super capacitor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108364794A true CN108364794A (en) | 2018-08-03 |
Family
ID=63006236
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810044071.XA Pending CN108364794A (en) | 2018-01-10 | 2018-01-10 | A kind of preparation method based on carbon cloth growth in situ tungstic acid electrode material for super capacitor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108364794A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110534350A (en) * | 2019-08-22 | 2019-12-03 | 江苏大学 | A kind of functionalized carbon nanometer sheet/WO3Nanometer rod composite material and preparation method |
| CN110838411A (en) * | 2019-11-19 | 2020-02-25 | 陕西科技大学 | Carbon cloth-loaded layered hexagonal tungsten trioxide supercapacitor electrode material and preparation method thereof |
| CN114927353A (en) * | 2022-02-16 | 2022-08-19 | 上海应用技术大学 | CF/WO 3 /TiO 2 Composite material and preparation and application thereof |
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| JP2010280551A (en) * | 2009-06-08 | 2010-12-16 | Kanto Denka Kogyo Co Ltd | Tungsten oxide fine particle and method for producing the same |
| CN102509635A (en) * | 2011-10-31 | 2012-06-20 | 华中科技大学 | Preparation method of flexible super capacitor based on carbon cloth |
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| CN105714377A (en) * | 2016-05-13 | 2016-06-29 | 青岛科技大学 | Method for preparing nanometer flower-shaped WO3 thin-film photo-anodes |
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-
2018
- 2018-01-10 CN CN201810044071.XA patent/CN108364794A/en active Pending
Patent Citations (6)
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110534350A (en) * | 2019-08-22 | 2019-12-03 | 江苏大学 | A kind of functionalized carbon nanometer sheet/WO3Nanometer rod composite material and preparation method |
| CN110534350B (en) * | 2019-08-22 | 2022-03-22 | 江苏大学 | Functionalized carbon nanosheet/WO3Nano-rod composite material and preparation method thereof |
| CN110838411A (en) * | 2019-11-19 | 2020-02-25 | 陕西科技大学 | Carbon cloth-loaded layered hexagonal tungsten trioxide supercapacitor electrode material and preparation method thereof |
| CN110838411B (en) * | 2019-11-19 | 2022-05-31 | 陕西科技大学 | Carbon cloth-loaded layered hexagonal tungsten trioxide supercapacitor electrode material and preparation method thereof |
| CN114927353A (en) * | 2022-02-16 | 2022-08-19 | 上海应用技术大学 | CF/WO 3 /TiO 2 Composite material and preparation and application thereof |
| CN114927353B (en) * | 2022-02-16 | 2024-01-26 | 上海应用技术大学 | CF/WO 3 /TiO 2 Composite material, preparation and application thereof |
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Address after: 266100 No. 308 Ningxia Road, Shinan District, Qingdao City, Shandong Province Applicant after: Qingdao University Address before: 266071 Ningxia Road, Shandong, China, No. 308, No. Applicant before: Qingdao University |
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Application publication date: 20180803 |