CN104681308A - Method for preparing aperture controllable three-dimensional microelectrode of super capacitor - Google Patents
Method for preparing aperture controllable three-dimensional microelectrode of super capacitor Download PDFInfo
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- CN104681308A CN104681308A CN201510122007.5A CN201510122007A CN104681308A CN 104681308 A CN104681308 A CN 104681308A CN 201510122007 A CN201510122007 A CN 201510122007A CN 104681308 A CN104681308 A CN 104681308A
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- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000003990 capacitor Substances 0.000 title abstract description 13
- 229920001486 SU-8 photoresist Polymers 0.000 claims abstract description 15
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 12
- 239000010703 silicon Substances 0.000 claims abstract description 12
- 238000003763 carbonization Methods 0.000 claims abstract description 9
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000004528 spin coating Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 8
- 229920002120 photoresistant polymer Polymers 0.000 claims description 7
- 238000003491 array Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052799 carbon Inorganic materials 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 abstract 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 abstract 3
- 238000010000 carbonizing Methods 0.000 abstract 1
- 238000012938 design process Methods 0.000 abstract 1
- 239000007787 solid Substances 0.000 abstract 1
- 239000007772 electrode material Substances 0.000 description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 229910000967 As alloy Inorganic materials 0.000 description 1
- 239000004966 Carbon aerogel Substances 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000011089 mechanical engineering Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- 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
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- 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
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention relates to the technical field of a micro electro mechanical system, in particular to a method for preparing an aperture controllable three-dimensional microelectrode of a super capacitor. The method comprises the following steps: firstly, doping FeCl3 solid particles of which the diameter is in the range of 2 to 50nm into SU-8 photoresist; then spin-coating the doped SU-8 photoresist on a silicon chip and obtaining a three-dimensional array structure with a vertical side wall and a high depth-to-width ratio by a photolithographic process; placing the structure into a high-temperature carbonization furnace to carry out carbonization to obtain a mesoporous carbon electrode. According to the method, from the angle of the design process, the specific surface area of the three-dimensional electrode is increased in a manner of doping FeCl3 into the SU-8 photoresist; FeCl3 is easy to directly sublimate at a high temperature and can be volatilized in the carbonizing process; mesoporous carbon most of which has the aperture range of 2 to 50nm is formed; the number of blind holes is reduced, and the utilization rate of the surface area of the porous carbon is greatly improved, so that the area of the electrode of the super capacitor is enlarged, and specific capacitance and specific power of the capacitor are improved.
Description
Technical field
The present invention relates to micro-electromechanical system field, be specially the ultracapacitor three-dimensional micro-electrode preparation method that a kind of aperture is controlled.
Background technology
MEMS (Micro Electro Mechanical Systems, i.e. microelectromechanical systems) 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, MEMS supercapacitor also shows while possessing conventional Super capacitor advantage that stored energy is large, volume microminiaturization, have extended cycle life, can the repeatedly feature such as cycle charge-discharge and batch production, reduce device volume and 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.
Ultracapacitor, according to the difference of energy storage mechnism, can be divided into double electric layer capacitor and fake capacitance capacitor, and the electrode material that wherein double electric layer capacitor uses mostly is porous carbon materials, such as active carbon, carbon aerogels, carbon nano-tube.The amount of capacity of double electric layer capacitor is relevant with the hole of electrode material.Usually, porosity is higher, and the specific area of electrode material is larger, and electric double layer capacitance is also larger.Simultaneously pore size can affect the utilance in hole, causes the movement rate of electrolyte ion to reduce or electrolyte ion cannot in access aperture due to the too small meeting in aperture, and aperture too conference makes space waste in hole.Therefore, how effectively to improve porosity, control pore size thus improve the Main way that the capacity of double electric layer capacitor becomes electrochemical capacitance research.
Summary of the invention
The present invention, in order to solve the little problem of double electric layer capacitor capacity, provides the ultracapacitor three-dimensional micro-electrode preparation method that a kind of aperture is controlled.
The present invention adopts following technical scheme to realize: the ultracapacitor three-dimensional micro-electrode preparation method that a kind of aperture is controlled, comprises the steps:
(1) choose silicon chip as substrate, will clean at the bottom of silicon wafer-based and dry;
(2) be the FeCl of 2-50nm by diameter
3evenly be incorporated in SU-8 photoresist, FeCl when mixing
3be 1:5 ~ 1:20 with the mass ratio of SU-8 photoresist;
(3) at the bottom of the silicon wafer-based after cleaning, drying, even spin coating is mixed with FeCl
3sU-8 photoresist;
(4) doped with FeCl
3to place figure be the mask plate of regular hexagon hole shape on SU-8 photoresist surface;
(5) SU-8 photoresist is exposed, developed, obtain three-dimensional regular hexahedron columnar arrays structure;
(6) the three-dimensional regular hexahedron columnar arrays structure obtained is put in retort carry out high temperature carbonization and obtain mesoporous carbon electrode.
The present invention proposes the controlled ultracapacitor three-dimensional micro-electrode preparation method in a kind of aperture.The FeCl that the method utilizes high temperature easily to distil
3the pore size of the effective control electrode material of particle, chooses the FeCl that diameter is 2-50nm in experiment
3as alloy, and with the quality of 1:5 ~ 1:20 than scope and the mixing of SU-8 photoresist, while guaranteeing electrode material porosity, effectively improve the specific area of electrode material, thus improve the ratio capacitance of double electric layer capacitor.Present invention incorporates SU-8 glue and FeCl
3superperformance, compared to common electrode material, the empty number that is situated between improves greatly, decreases the quantity of blind hole, significantly improves the surface area utilance of electrode material, finally reaches the object improving ratio capacitance and specific energy.
The ultracapacitor three-dimensional micro-electrode preparation method that above-mentioned a kind of aperture is controlled, in carbonization process, temperature, the rate of heat addition and cooldown rate arrange as follows: first, and temperature is elevated to 450 DEG C from room temperature by used time 130min, stablizes 60min; Temperature is risen to 700 DEG C by used time 100min again, and heating rate is 2.5 DEG C/minute, stablizes 90min; Need 80min to be warming up to 900 DEG C afterwards again, heating rate is 2.5 DEG C/minute, continues to stablize 60min; Final used time 40min is warming up to 1000 DEG C, and heating rate is 2.5 DEG C/minute, continual and steady 60min, progressively completes the charing completely of array structure; Naturally cool 360min and be down to room temperature.Carbonization temperature is multi-level ladder propradation, and one is to fully carbonize at a certain temperature, is conducive to the eliminating of specific product at this temperature, increases the mesoporous quality and quantity of electrode; Two is slow down heating rate can reduce the different problem causing electrode to come off from silicon base of the coefficient of expansion with cooldown rate, utilizes and increases the specific area that mesoporous quality and quantity increases electrode.
Present invention achieves the control to porous carbon aperture, improve porous surface and amass utilance.Thus reach the object increasing specific capacity of double-layer capacitor and specific power.Processing technology in the present invention is simple to operation.Size is little, and quality is light, can be integrated, is widely used in the Power supply of micro mechanical system.
Accompanying drawing explanation
Fig. 1 is electrode structure vertical view.
Fig. 2 is carbonization temperature time plot.
Embodiment
(1) choose 2 cun of silicon chips as substrate, and clean at the bottom of silicon wafer-based with wipe oil, oxide-film and metal ion in dimethylbenzene, acetone, alcohol, sulfuric acid/hydrogen peroxide, ammoniacal liquor/hydrogen peroxide, hydrochloric acid/hydrogen peroxide solution successively, then dry;
(2) be the FeCl of 2-50nm by diameter
3be incorporated in SU-8 photoresist, FeCl when mixing
3be 1:5 ~ 1:20 with the mass ratio of SU-8 photoresist, use magnetic stirrer to stir and make it mix;
(3) at the bottom of the silicon wafer-based after cleaning, drying by twice lacquering technique spin coating thickness be 500 μm doped with FeCl
3sU-8 photoresist, before whirl coating, first will be heated to 45 DEG C at the bottom of silicon wafer-based, then carry out first time whirl coating, first time whirl coating complete after first to photoresist carry out certain hour front baking solidification, carry out second time whirl coating afterwards;
(4) by the close contact post-exposure of photoresist surface with mask plate, the time for exposure is 120s, then puts into baking oven by the bottom of silicon wafer-based, is warming up to 60 DEG C, keeps 1min, is warming up to 90 DEG C, keeps 30min, takes out after naturally cooling to room temperature; Then photoresist is placed on photoresist developing 60min under ultrasonic environment, obtains column hexahedron structure;
(5) three-dimensional regular hexahedron columnar arrays structure is put in retort, carry out in the environment of 95% nitrogen/5% hydrogen during charing, in carbonization process, temperature, the rate of heat addition and cooldown rate arrange as follows: first, and temperature is elevated to 450 DEG C from room temperature by used time 130min, stablizes 60min; Temperature is risen to 700 DEG C by used time 100min again, and heating rate is 2.5 DEG C/minute, stablizes 90min; Need 80min to be warming up to 900 DEG C afterwards again, heating rate is 2.5 DEG C/minute, continues to stablize 60min; Final used time 40min is warming up to 1000 DEG C, and heating rate is 2.5 DEG C/minute, continual and steady 60min, progressively completes the charing completely of array structure; Naturally cool 360min and be down to room temperature, final charing obtains mesoporous carbon electrode.
Claims (2)
1. the ultracapacitor three-dimensional micro-electrode preparation method that aperture is controlled, is characterized in that comprising the steps:
(1) choose silicon chip as substrate, will clean at the bottom of silicon wafer-based and dry;
(2) be the FeCl of 2-50nm by diameter
3evenly be incorporated in SU-8 photoresist, FeCl when mixing
3be 1:5 ~ 1:20 with the mass ratio of SU-8 photoresist;
(3) at the bottom of the silicon wafer-based after cleaning, drying, even spin coating is doped with FeCl
3sU-8 photoresist;
(4) doped with FeCl
3to place figure be the mask plate of regular hexagon hole shape on SU-8 photoresist surface;
(5) SU-8 photoresist is exposed, developed, obtain three-dimensional regular hexahedron columnar arrays structure;
(6) the three-dimensional regular hexahedron columnar arrays structure obtained is put in retort carry out high temperature carbonization and obtain mesoporous carbon electrode.
2. the ultracapacitor three-dimensional micro-electrode preparation method that a kind of aperture according to claim 1 is controlled, it is characterized in that temperature in carbonization process, the rate of heat addition and cooldown rate are arranged as follows: first, temperature is elevated to 450 DEG C from room temperature by used time 130min, stablizes 60min; Temperature is risen to 700 DEG C by used time 100min again, and heating rate is 2.5 DEG C/minute, stablizes 90min; Need 80min to be warming up to 900 DEG C afterwards again, heating rate is 2.5 DEG C/minute, continues to stablize 60min; Final used time 40min is warming up to 1000 DEG C, and heating rate is 2.5 DEG C/minute, continual and steady 60min, progressively completes the charing completely of array structure; Naturally cool 360min and be down to room temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510122007.5A CN104681308A (en) | 2015-03-20 | 2015-03-20 | Method for preparing aperture controllable three-dimensional microelectrode of super capacitor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510122007.5A CN104681308A (en) | 2015-03-20 | 2015-03-20 | Method for preparing aperture controllable three-dimensional microelectrode of super capacitor |
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|---|---|
| CN104681308A true CN104681308A (en) | 2015-06-03 |
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|---|---|---|---|
| CN201510122007.5A Pending CN104681308A (en) | 2015-03-20 | 2015-03-20 | Method for preparing aperture controllable three-dimensional microelectrode of super capacitor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105675682A (en) * | 2015-12-28 | 2016-06-15 | 中国人民大学 | Size-controllable nanowire microelectrode, preparation method and application thereof |
| CN108807007A (en) * | 2018-08-08 | 2018-11-13 | 武汉理工大学 | The manufacture craft of three-dimensional manometer threadiness hole carbon material and high voltage micro super capacitor |
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| CN1702887A (en) * | 2005-05-20 | 2005-11-30 | 清华大学 | Process for preparing carbon electrode array with high surface area and high gap filling capacity |
| US20080176138A1 (en) * | 2007-01-19 | 2008-07-24 | Park Benjamin Y | Carbon electrodes for electrochemical applications |
| CN101388291A (en) * | 2008-10-31 | 2009-03-18 | 中国科学院上海硅酸盐研究所 | Boron containing porous carbon electrode material and preparation thereof |
| CN101421866A (en) * | 2004-02-11 | 2009-04-29 | 加州大学评议会 | High aspect ratio C-MEMS architecture |
| CN103588165A (en) * | 2013-11-27 | 2014-02-19 | 华中科技大学 | Three dimensional trans-scale charcoal electrode array structure and manufacture method |
-
2015
- 2015-03-20 CN CN201510122007.5A patent/CN104681308A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101421866A (en) * | 2004-02-11 | 2009-04-29 | 加州大学评议会 | High aspect ratio C-MEMS architecture |
| CN1702887A (en) * | 2005-05-20 | 2005-11-30 | 清华大学 | Process for preparing carbon electrode array with high surface area and high gap filling capacity |
| US20080176138A1 (en) * | 2007-01-19 | 2008-07-24 | Park Benjamin Y | Carbon electrodes for electrochemical applications |
| CN101388291A (en) * | 2008-10-31 | 2009-03-18 | 中国科学院上海硅酸盐研究所 | Boron containing porous carbon electrode material and preparation thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105675682A (en) * | 2015-12-28 | 2016-06-15 | 中国人民大学 | Size-controllable nanowire microelectrode, preparation method and application thereof |
| CN105675682B (en) * | 2015-12-28 | 2019-03-26 | 中国人民大学 | A kind of nano wire microelectrode and the preparation method and application thereof that size is controllable |
| CN108807007A (en) * | 2018-08-08 | 2018-11-13 | 武汉理工大学 | The manufacture craft of three-dimensional manometer threadiness hole carbon material and high voltage micro super capacitor |
| CN108807007B (en) * | 2018-08-08 | 2019-10-25 | 武汉理工大学 | The manufacture craft of three-dimensional manometer threadiness hole carbon material and high voltage micro super capacitor |
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Application publication date: 20150603 |