CN104681304A - Preparation method of asymmetric supercapacitor - Google Patents
Preparation method of asymmetric supercapacitor Download PDFInfo
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- CN104681304A CN104681304A CN201510122091.0A CN201510122091A CN104681304A CN 104681304 A CN104681304 A CN 104681304A CN 201510122091 A CN201510122091 A CN 201510122091A CN 104681304 A CN104681304 A CN 104681304A
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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
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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
- H01G11/04—Hybrid capacitors
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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
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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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
- H01G11/32—Carbon-based
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
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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
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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 relates to the technical field of micro electromechanical systems, in particular to a preparation method of an asymmetric supercapacitor. The preparation method comprises the following steps: firstly preparing two identical cleaned and dried silicon wafer substrates; oxidizing the surface of one of the silicon wafer substrates to form a silicon dioxide insulating layer, and depositing a metallic titanium layer; anodizing to form an ordered TiO2 nanotube; depositing NiO in the TiO2 nanotube to prepare a TiO2 nanotube electrode; uniformly spinning SU-8 adhesive on the other silicon wafer substrate, performing photoetching on the SU-8 adhesive to form a hexahedron cylindrical array structure, and carbonizing the array structure so as to obtain the carbonized electrode; at last using a PP film to isolate the TiO2 nanotube electrode from the carbonized electrode, filling electrolyte into the electrodes, and assembling the electrodes to form the asymmetric supercapacitor. According to the preparation method disclosed by the invention, the Faradaic pseudocapacitance theory and the double layer theory are comprehensively utilized; the two prepared electrodes are both provided with porous structures; compared with the conventional supercapacitor, the specific capacitance of the supercapacitor based on the double layer theory can be improved.
Description
Technical field
The present invention relates to MEMS (micro electro mechanical system) (Micro Electro Mechanical System MEMS) technical field, belong to the manufacturing technology scope of micro super capacitor, be specially a kind of Asymmetric Supercapacitor preparation method.
Background technology
MEMS (Micro Electromechanical System, i.e. MEMS (micro electro mechanical system)) be a kind of industrial technology that microelectric technique and mechanical engineering are fused together, it has, and cost is low, volume is little, automatic control strong, high reliability, is one of most important technological innovation in recent years.
Ultracapacitor is a kind of novel energy storage device, with features such as the Large Copacity of its uniqueness, big current, fast charging and discharging and high service life cycles, is subject to the favor of common people, causes many Novel super capacitor be in succession developed and apply.MEMS supercapacitor also show while possessing conventional Super capacitor advantage can realize device microminiaturization, intellectuality and integrated, substantially increase device energy storage density; Simplify supercapacitor structures design, matched design device chip control circuit condition of work better, reduce device volume, reduce design cost; Improve the reliability and stability of device layout system.Therefore MEMS supercapacitor is subject to showing great attention to of domestic and international researcher.But the energy density of MEMS supercapacitor is low, the energy density therefore how improving micro super capacitor becomes a Main way of electrochemical capacitance research.
Ultracapacitor, according to the difference of energy storage mechnism, can be divided into double electric layer capacitor and Faradic pseudo-capacitor.Double electric layer capacitor utilizes the interfacial electric double layer electric capacity formed between electrode and electrolyte to carry out stored energy, and its electrode adopts the porous carbon materials with high-specific surface area usually, has higher ratio capacitance; Faradic pseudo-capacitor refer to electrode surface or body mutually in two dimension or accurate two-dimensional space on, electrode active material carries out underpotential deposition, make it that quick, reversible chemisorbed/desorption or oxidation/reduction reaction occur, thus producing the specific capacity higher than double electric layer capacitor, its electrode material is metal oxide and conducting polymer mainly.But no matter all cannot meet the requirement of energy density and power density based on the ultracapacitor of certain single principle simultaneously, in order to obtain higher energy density and power density simultaneously, people start to design novel non-symmetrical electrochemical supercapacitor, namely a pole of capacitor is double layer electrodes, and another is pseudo capacitance electrode very.Non-symmetrical electrochemical supercapacitor combines the advantage of two class electrochemical capacitors, effectively can break through the limitation that general ultracapacitor cannot meet energy density and power density simultaneously, the overall requirement to the energy density of power-supply system and power density of load in practical application can be met better.Constantly applied in fields such as mobile communication, information technology, Aero-Space and science and techniques of defence.But the capacitance of existing non-symmetrical electrochemical supercapacitor or little, can not meet practical application completely.
Summary of the invention
The present invention, in order to the little problem of the capacitance that solves existing non-symmetrical electrochemical supercapacitor, provides a kind of Asymmetric Supercapacitor preparation method.
The present invention adopts following technical scheme to realize: a kind of Asymmetric Supercapacitor preparation method, comprises the following steps:
S1: choose two panels silicon chip as substrate, cleaning silicon chip substrate is also dried;
S2: be oxidized at the bottom of the silicon wafer-based after cleaning, drying, forms the insulating barrier of silicon dioxide oxide-film as electrode at silicon wafer-based basal surface;
S3: the surface at the bottom of the wherein a slice silicon wafer-based forming insulating barrier forms layer of metal titanium layer by deposition;
S4: the titanium layer formed in S3 is put into anodic oxidation device and is oxidized, forms TiO
2nanotube;
S5: the TiO formed
2in nanotube, deposition NiO, forms TiO
2nanotube electrode;
S6: even spin coating photoresist on another silicon chip of the surface formation insulating barrier obtained in S2;
S7: photoresist good for spin coating is carried out front baking, exposure, rear baking, development treatment, forms hexahedron columnar arrays;
S8: hexahedron columnar arrays is put into retort and carbonizes, obtains carbonizing electrode;
S9: active material electrode and charing electrode are separated by PP film, and injects KOH electrolyte and be assembled into Asymmetric Supercapacitor.
Above-mentioned a kind of Asymmetric Supercapacitor preparation method, comprises the following steps: be oxidized to dry-oxygen oxidation or wet-oxygen oxidation at the bottom of silicon wafer-based, and the thickness of insulating layer of formation is 1.5 microns.Can prevent silicon base from contacting with electrode, form short circuit.
Above-mentioned a kind of Asymmetric Supercapacitor preparation method, titanium layer thickness is 400nm.Because thickness is moderate, can avoid that titanium layer is oxidized to be penetrated.
Above-mentioned a kind of Asymmetric Supercapacitor preparation method, anodic oxidation electrolyte is the HF aqueous solution of 0.05wt%, oxidizing process middle-jiao yang, function of the spleen and stomach very Ti electrode, and negative electrode is the TiO of platinum electrode, formation
2the thickness of nanotube is 150nm.With this understanding, the TiO of formation
2nanotube alignment is regular, and density is high, and controllability is strong.
Above-mentioned a kind of Asymmetric Supercapacitor preparation method, described in be deposited as constant current electro-deposition, the time is 20 minutes.The metallic nickel sedimentary deposit of uniform thickness can be generated on TiO2 nano-tube support.
A kind of Asymmetric Supercapacitor preparation method of deposit those, described photoresist is negative glue SU-8, and spin coating thickness is 200 microns.Thickness is thicker, and the well table area formed afterwards in charing is larger, and after forming electrode, corresponding ratio capacitance can increase.
The present invention proposes Asymmetric Supercapacitor three-dimensional micro-electrode preparation method, the method utilizes two electrodes all to form loose structure to increase the surface area of electrode, simultaneously, negative pole SU-8 glue used is due to good mechanical property, so the hole vertical sidewall formed after charing is good, further increase the ratio capacitance of ultracapacitor.In process, involved anodic oxidation and carbonization process simple possible, precision is high, and be easy to operation, cost of investment is not high.Because ultracapacitor has the power density higher than conventional batteries, and the Asymmetric Supercapacitor that the present invention proposes wherein adopts faraday's " pseudo-capacitance " energy storage principle in a pole, significantly increase the energy density of capacitor, the obstacle that common super capacitor energy density and power density can not get both can be efficiently solved, be with a wide range of applications.
Accompanying drawing explanation
Fig. 1 is TiO
2nanotube electrode preparation technology flow chart.
Fig. 2 is TiO
2vertical view at the bottom of silicon wafer-based in nanotube electrode preparation technology.
Fig. 3 is charing technology for preparing electrode flow chart.
Fig. 4 is vertical view at the bottom of silicon wafer-based in charing technology for preparing electrode.
Fig. 5 is Asymmetric Supercapacitor three-dimensional micro-electrode global design figure.
Embodiment
A kind of Asymmetric Supercapacitor preparation method, comprises the following steps:
S1: choose two panels 2cm × 2cm silicon chip as substrate, clean with wipe oil in hydrogen peroxide, sulfuric acid/hydrogen peroxide, hydrochloric acid/ammonia, hydrogen peroxide solution successively at the bottom of silicon wafer-based, oxide-film and metal ion, then dry;
S2: be oxidized putting in oxidation furnace at the bottom of the silicon wafer-based after cleaning, drying, mode of oxidizing is dry oxidation or wet-oxygen oxidation, oxidation duration is 5 hours, and form the insulating barrier of silicon dioxide oxide-film as electrode at silicon wafer-based basal surface, thickness of insulating layer is 1.5 microns;
S3: will be placed in depositing system device at the bottom of wherein a slice silicon wafer-based of formation insulating barrier, at silicon wafer-based basal surface by depositional mode plated metal titanium layer, its thickness be 400nm;
S4: the titanium layer formed in S3 is put into anodic oxidation device and is oxidized, anodic oxidation electrolyte is the HF aqueous solution of 0.05wt%, oxidizing process middle-jiao yang, function of the spleen and stomach very Ti electrode, negative electrode is platinum electrode, first apply 10V voltage 20 seconds during oxidation, then 0.5V voltage 30 minutes, form TiO
2nanotube, the TiO of formation
2nano aperture thickness is 150nm;
S5: the TiO first formed by Constant Electric Current deposition
2plated metal Ni in nanotube, then be oxidized by cyclic voltammetry, generate the oxide nickel hydroxide of W metal, then obtain NiO with high temperature dehydration process, complete TiO
2the preparation of nanotube electrode;
S6: on another silicon chip of the surface formation insulating barrier obtained in S2, evenly glue SU-8 photoresist is born in spin coating, spin coating thickness is 200 microns, wherein photoresist need carry out front baking process, to remove the solvent in photoresist, play the effect that silicon face fixes photoresist, pre-bake temperature is 65 DEG C, and the time is 10 minutes;
S7: photoresist is carried out mask exposure, the time for exposure is 15s; Then carry out rear baking, rear baking temperature is 95 DEG C, and the time is half an hour; Develop afterwards, develop 15 minutes in acetone developer solution, obtain hexahedron columnar arrays;
S8: the hexahedron columnar arrays of gained is put into retort charing 24 hours, obtains carbonizing electrode;
S9: active material electrode and charing electrode are separated by PP film (polypropylene screen), notes and be assembled into Asymmetric Supercapacitor with KOH electrolyte.
Claims (6)
1. an Asymmetric Supercapacitor preparation method, is characterized in that comprising the following steps:
S1: choose two panels silicon chip as substrate, cleaning silicon chip substrate is also dried;
S2: be oxidized at the bottom of the silicon wafer-based after cleaning, drying, forms the insulating barrier of silicon dioxide oxide-film as electrode at silicon wafer-based basal surface;
S3: the surface at the bottom of the wherein a slice silicon wafer-based forming insulating barrier forms layer of metal titanium layer by deposition;
S4: the titanium layer formed in S3 is put into anodic oxidation device and is oxidized, forms TiO
2nanotube;
S5: the TiO formed
2in nanotube, deposition NiO, forms TiO
2nanotube electrode;
S6: even spin coating photoresist on another silicon chip of the surface formation insulating barrier obtained in S2;
S7: photoresist good for spin coating is carried out front baking, exposure, rear baking, development treatment, forms hexahedron columnar arrays;
S8: hexahedron columnar arrays is put into retort and carbonizes, obtains carbonizing electrode;
S9: active material electrode and charing electrode are separated by PP film, and injects KOH electrolyte and be assembled into Asymmetric Supercapacitor.
2. a kind of Asymmetric Supercapacitor preparation method according to claim 1, is characterized in that comprising the following steps: be oxidized to dry-oxygen oxidation or wet-oxygen oxidation at the bottom of silicon wafer-based, and the thickness of insulating layer of formation is 1.5 microns.
3. a kind of Asymmetric Supercapacitor preparation method according to claim 1 and 2, is characterized in that titanium layer thickness is 400nm.
4. a kind of Asymmetric Supercapacitor preparation method according to claim 1 and 2, it is characterized in that anodic oxidation electrolyte is the HF aqueous solution of 0.05wt%, oxidizing process middle-jiao yang, function of the spleen and stomach very Ti electrode, negative electrode is platinum electrode, and the thickness of the TiO2 nanotube of formation is 150nm.
5. a kind of Asymmetric Supercapacitor preparation method according to claim 1 and 2, is deposited as constant current electro-deposition described in it is characterized in that, the time is 20 minutes.
6. a kind of Asymmetric Supercapacitor preparation method according to claim 1 and 2, it is characterized in that described photoresist is for negative glue SU-8, spin coating thickness is 200 microns.
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| CN201510122091.0A CN104681304B (en) | 2015-03-20 | 2015-03-20 | A kind of Asymmetric Supercapacitor preparation method |
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Cited By (3)
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| CN105448536A (en) * | 2015-11-26 | 2016-03-30 | 合肥工业大学 | Nickel oxide/titanium oxide nanocomposite and preparation method and energy storage application therefor |
| CN106340445A (en) * | 2016-09-13 | 2017-01-18 | 复旦大学 | Manufacturing method of two-dimensional ordered TiO2 nanometer well film and application in self-energized photoelectric device |
| CN107346712A (en) * | 2017-07-24 | 2017-11-14 | 淮海工学院 | A kind of flexible and transparent ultracapacitor based on micro-nano technology technology |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN106340445A (en) * | 2016-09-13 | 2017-01-18 | 复旦大学 | Manufacturing method of two-dimensional ordered TiO2 nanometer well film and application in self-energized photoelectric device |
| CN106340445B (en) * | 2016-09-13 | 2019-10-15 | 复旦大学 | Sequential 2 D TiO2The preparation method of nanometer well film and the application in self energizing photoelectric device |
| CN107346712A (en) * | 2017-07-24 | 2017-11-14 | 淮海工学院 | A kind of flexible and transparent ultracapacitor based on micro-nano technology technology |
| CN107346712B (en) * | 2017-07-24 | 2019-03-12 | 淮海工学院 | A kind of flexible and transparent supercapacitor based on micro-nano technology technology |
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| CN104681304B (en) | 2017-08-25 |
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