CN101504889A - Micro super capacitor applied for micro system and production process thereof - Google Patents
Micro super capacitor applied for micro system and production process thereof Download PDFInfo
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- CN101504889A CN101504889A CN 200910079670 CN200910079670A CN101504889A CN 101504889 A CN101504889 A CN 101504889A CN 200910079670 CN200910079670 CN 200910079670 CN 200910079670 A CN200910079670 A CN 200910079670A CN 101504889 A CN101504889 A CN 101504889A
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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 discloses a micro supercapacitor applied to a micro system and a preparation method thereof, which belong to the manufacturing technology range of miniature supercapacitors. The preparation method comprises the following steps: drawing graphs of a micro capacitor and an array thereof on a silicon substrate through a mask and a photoetching method; preparing a layer of a metal film current collector and a layer of a ruthenium-oxide film cathode layer on the silicon substrate; spin-coating a layer of a polyimide sacrifice layer on the layers to obtain a required support body structure and a peripheral liquid storage cavity enclosure structure; spin-coating the sacrifice layer on the layers again and depositing an anode ruthenium-oxide active substance layer and a nickel film current collector layers in turn on the layers; perforating filling holes on the upper nickel layer and an oxide layer to fill an electrolyte in a cavity; and finally, covering a polymer film layer on the whole micro supercapacitor array again to finish an encapsulation process. The micro supercapacitor is provided with the unique support body structure and the liquid storage cavity structure, has the characteristics of small volume, large energy storage density, high discharge power, monolithic and the like, can be manufactured in batches, and has wide application prospect.
Description
Technical field
The invention belongs to the manufacturing technology scope of micro super capacitor, particularly based on a kind of micro super capacitor that is applied to micro-system of the active microelectrode of ruthenium-oxide and preparation method thereof.
Background technology
Miniaturization of electronic products, microminiaturization, integrated be the trend of the times of world today's technical development.Microelectromechanical systems (Micro Electro Mechanical Systems is called for short MEMS) has mobility, automatic control, characteristics such as integrated, is one of most important technological innovation in recent years.When a subsystem can be integrated on the chip piece, power supply also must be finished the revolution of miniaturization, microminiaturization.The MEMS micro-energy resource system is meant the technology based on MEMS, it is that micron order, overall dimension are the micro-system of Centimeter Level that one or more electric energy feedwaies are integrated into a characteristic size, can realize long-time, high-effect, multi-mode power supply, be specially adapted to some particular surroundings that conventional power source can't be used.The miniature energy of excellent performance is to the development of MEMS system and improve and just have special meaning.At first, the miniature energy of integrated independence can effectively solve the technical barrier of the serious dependence externally fed in present puzzlement microsystems technology field.The second, the miniature energy of Highgrade integration can improve the energy conversion efficiency of system greatly, has farthest reduced the energy loss of system.The 3rd, the integrated miniature energy is the simplified system external circuit greatly, effectively reduces whole micro-system cost.At present the patent in external this field mainly concentrates on fields such as miniature lithium ion battery, micro zinc-nickel battery, as the patent (US.6610440BS) of the relevant micro zinc-nickel battery of the patent (US.5567210) of the relevant miniature lithium ion battery of U.S. oak ridge National Laboratory and U.S. Bipolar technologies company.Up to the present, the report of relevant micro super capacitor seldom, U.S. TPL company uses ruthenium-oxide/carbon aerosol combination electrode material and MEMS technology to prepare micro super capacitor (US6621687 B2), two kinds of capacitors of difference according to electrolyte have the operating voltage of 1V and 2.5V respectively, form the high power discharge problem that composite power source can effectively solve the MEMS system with the miniature lithium ion battery that the said firm develops.Be pointed out that the technology of U.S. TPL company is at first to prepare the micro super capacitor individuality, and then it is installed in the MEMS system, and often resistance is bigger to adopt the method that applies slurry to prepare electrode.This patent proposes a kind of micro super capacitor based on the MEMS technology, be in the ultracapacitor preparation process, to introduce the microminiature electronic devices and components that the MEMS technology is finished, designs has unique supporting body structure and cavity liquid storage structure, device has that volume is little, discharge power is high, singualtion, characteristics such as can make in batches, has widely in fields such as microelectric technique, fuse technology, wireless sensor network technologies and uses.
Summary of the invention
The objective of the invention is to propose a kind of a kind of micro super capacitor that is applied to micro-system based on the MEMS technology and preparation method thereof, the structure of described micro super capacitor and processing process are: preparation one deck thin nickel metal film collector 2 and ruthenium-oxide film 5 on silicon substrate 1, on the ruthenium-oxide active film 5 be supporting body structure 3 and liquid storage cavity fence structure 4 between electrode, on supporting body structure between electrode 3, prepare ruthenium-oxide film 5 again, at liquid storage cavity fence structure 4, be liquid storage cavity 6 between supporter 3 and the ruthenium-oxide film 5 between electrode, on whole micro super capacitor array, cover polyimides encapsulated layer 7 once more at last.
The processing process of described micro super capacitor is: the figure of drawing out microcapacitor and array thereof by the method or the photoetching method of mask on silicon substrate 1 prepares one deck thin nickel metal film collector 2 and ruthenium-oxide film 5 thereon then as positive active material.Spin coating one deck polyimide sacrificial layer once more on ruthenium-oxide active film 5 obtains supporting body structure 3 and liquid storage cavity fence structure 4 on every side by photoetching, developing procedure.Said structure is carried out the high-temperature sub amination treatment so that supporting body structure 3 and liquid storage cavity fence structure 4 obtain high structural strength and corrosion-resistant; Spin coating sacrifice layer and deposit ruthenium-oxide film 5 thereon successively as negative electrode active material layer once more after finishing imidization and handling is got liquid injection hole on negative electrode active material layer, discharge the polyimide sacrificial layer in the middle of the positive and negative electrode; In the cavity that forms, pour into electrolyte then, on whole micro super capacitor array, cover the polyimides rete once more at last to finish encapsulation process.
Described micro super capacitor adopts " liquid storage cavity between electrode " structure to replace traditional " electrode diaphragm stack " structure.This liquid storage cavity structure has been removed conventional membrane fully, and the setting by liquid storage cavity between microelectrode reaches the raising electrode activity, reduces the purpose of internal resistance between electrode.Unique " liquid storage cavity structure between electrode " reduces micro element processing technology complexity greatly, is convenient to preparation in enormous quantities, can effectively solve " electrode diaphragm laminated construction " intrinsic some technical barriers.
The described graphics art of drawing out microcapacitor and array thereof is: preparation one deck SiO on silicon substrate
2Or spin coating one deck light-sensitive polyimide photoresist is as the sacrifice layer of metallic films such as preparation nickel, the figure of drawing out microcapacitor and array thereof by the method or the photoetching method of mask thereon.
The technology of preparing route of described nickel-base anode collector and ruthenium-oxide active material is: adopt evaporation, sputtering method to prepare one deck thin nickel metal film as collector on the figure of array, use the anodal layers of prepared ruthenium-oxide film such as vapour deposition CVD on the nickel collector.
The technology of preparing route of supporter and liquid storage cavity structure is between described positive and negative electrode: spin coating one deck polyimide sacrificial layer once more on the ruthenium-oxide active material layer obtains needed supporting body structure and liquid storage cavity fence structure on every side by uv-exposure photoetching, developing procedure.Supporting body structure is carried out the high-temperature sub amination treatment to obtain supporter and liquid storage cavity enclosure wall between high structural strength and corrosion resistant electrode.
The technology of preparing route of described negative pole ruthenium-oxide active material and nickel collector is: spin coating sacrifice layer and adopt with anodal similarly method and deposit negative pole ruthenium-oxide active material layer and nickel film current collector layers thereon successively once more after finishing above-mentioned supporter and cavity structure and handling.
The technology of preparing route of electrolyte liquid storage cavity is between described both positive and negative polarity: get conversion and the thoroughly release of micro through-hole array to make things convenient for the polyimide sacrificial layer material on capacitor package layer and ruthenium-oxide/nickel negative electrode layer.Adopt the reactive plasma lithographic method that the polyimide sacrificial layer between both positive and negative polarity and oxygen reaction are formed carbon monoxide and these volatile substances of water then and finally discharge.In cavity, inject potassium hydroxide electrolyte and hole is shut back micro super capacitor preparation technology finish.
The invention has the beneficial effects as follows the technical scheme that this micro super capacitor has adopted supporter micro-structural, liquid storage cavity micro-structural to combine with little active electrode preparation, effectively reduce electrode gap, improve little energy accumulate performance, strengthen the high power discharge ability of little energy device.Compare with solid electrolyte, the mobile liquid electrolyte in the liquid storage cavity has advantages such as activity is high, internal resistance is low.The present invention is expected in the acquisition extensive use of fields such as microelectric technique, fuse technology, wireless sensor network technology.Described micro super capacitor is based on the preparation of MEMS technology and is applied to the miniature energy storage device of micro-system, its objective is the independently-powered problem of researching and solving MEMS (micro electro mechanical system) inside by relevant little energy technology.
Description of drawings
Fig. 1 is the structural representation of micro super capacitor.
Embodiment
The present invention proposes a kind of micro super capacitor that is applied to micro-system and manufacture method thereof based on the MEMS micro-processing technology.Described micro super capacitor adopts supporter and liquid storage cavity space structure between unique electrode, by ruthenium-oxide positive and negative electrode and KOH electrolyte be sealed in constitute in the polyimides encapsulated layer have that volume is little, energy storage density is big, discharge power is high, the micro super capacitor of characteristics such as simple in structure, easy to process, dependable performance.
Figure 1 shows that the space structure schematic diagram of micro super capacitor.The structure of micro super capacitor described in the figure and processing process are: preparation one deck thin nickel metal film collector 2 and ruthenium-oxide film 5 on silicon substrate 1, on the ruthenium-oxide active film 5 be supporting body structure 3 and liquid storage cavity fence structure 4 between electrode, on supporting body structure between electrode 3, prepare ruthenium-oxide film 5 again, at liquid storage cavity fence structure 4, be liquid storage cavity 6 between supporter 3 and the ruthenium-oxide film 5 between electrode, on whole micro super capacitor array, cover polyimides encapsulated layer 7 once more at last.
Packaging technology of the present invention specifies as follows;
1. the anodal Ni-based collector of micro super capacitor graphically prepares
Described micro super capacitor adopts silicon chip as substrate,, it is 0.3～1 micron SiO that one side prepares thickness with thermal oxidation method
2Insulating barrier, spin coating 30 microns～80 micron thickness light-sensitive polyimide photoresists and adopt the ultraviolet photoetching lithographic technique to form required pattern thereon on insulating barrier.Above photoresist, adopt RF sputtering method sputter Cr layer and Ni layer successively, the thickness of Cr-Ni composite bed is subjected to the photoresist thickness limits, thickness range is 10 microns～30 microns, the purpose of sputter Cr metal level be make contact between Ni metal level and the silicon substrate more firm.Also can adopt vacuum electron beam evaporation coating method to prepare above-mentioned Cr-Ni metal composite layer.Leave 30 microns～50 micron thickness spaces between prepared metal composite laminar surface and the thick film surface and be used to deposit the ruthenium-oxide active material.
2. the anodal ruthenium-oxide active material preparation of micro super capacitor
Adopt high-purity ruthenium metal as target, at ambient temperature, in argon gas/oxygen atmosphere, carry out reactive sputtering and prepare the ruthenium-oxide active material layer.Deposition ruthenium-oxide active material layer thickness is 30 microns～50 microns, and ruthenium-oxide active material laminar surface should not be higher than peripheral photoresist mask surface.After finishing the active material layer preparation the above-mentioned silicon chip that is loaded with photoresist and metal is dipped in the chlorobenzene developer solution that can dissolve photoresist, directly is deposited on SiO
2Lip-deep microelectrode array will be retained, and the nickel metal and the ruthenium-oxide active material that are deposited on the photoresist will come off from substrate along with the dissolving of photoresist.
3. supporter and liquid storage cavity enclosure wall preparation between the micro super capacitor electrode
After the deposition preparation of ruthenium-oxide active material layer is finished, the thick glue of spin coating light-sensitive polyimide once more on the electrod-array plane, the photoresist thickness of this operation spin coating is 100～150 microns.Further adopt the uv-exposure pattern technology at ruthenium-oxide electrode surface preparation supporting body structure, prepare the liquid storage cavity fence structure at electrode edge.Then the above-mentioned silicon chip that is loaded with photoresist and metal is dipped in the chlorobenzene developer solution that can dissolve photoresist, splits away off through the photoresist dissolving of sensitizationization after the exposure-processed and from substrate.Light-sensitive polyimide supporter and fence structure need the high-temperature sub amination more than 150 ℃ after photoetching formation, to guarantee that good mechanical property is arranged.The polyimides after the imidization and the bond strength of ruthenium-oxide are very high, and tensile strength and compression strength are all bigger, can satisfy the demand as supporter.
4. micro super capacitor negative pole ruthenium-oxide active material preparation
On the structure sheaf surface of finishing the preparation of supporter and fence structure once more the spin-on polyimide photoresist as the further sacrifice layer material of preparation cavity structure, photoresist thickness is no more than supporter and enclosure wall height, also can adopt the polymer poly methyl methacrylate as sacrifice layer.Adopt high-purity ruthenium metal as target on the photoresist surface once more, in room temperature and argon gas/oxygen atmosphere, carry out reactive sputtering and prepare the ruthenium-oxide negative electrode active material layer.Ruthenium-oxide active material layer thickness is 30 microns～50 microns.Adopt nickel as target then, as collector, thickness is 10 microns～20 microns at ruthenium-oxide negative electrode active material layer surface sputtering nickel dam, at last spin coating one deck thick polyimide film encapsulated layer once more on the nickel dam surface.
5. the micro super capacitor liquid storage cavity prepares and perfusion electrolyte
For discharging sacrifice layer material between electrode completely, adopt laser boring method on capacitor package layer and ruthenium-oxide/nickel negative electrode layer, to get of conversion and the thoroughly release of micro through-hole array to make things convenient for the polyimide sacrificial layer material by thermal effect.Adopt the reactive plasma lithographic method that polyimide sacrificial layer between both positive and negative polarity and oxygen reaction are formed volatile substances such as carbon monoxide and water then, finally from micro channel, discharge.Usually can produce internal stress in thin film deposition process, after sacrifice layer was removed, the internal stress of superstructure will discharge, thereby produced distortion.Generally come proof stress by process conditions such as control sacrifice layer reaction speeds.The reactive plasma etching is compared with wet etching, and obviously advantage is exactly that control easily and plasma etching have very high anisotropy, and directivity is very strong, for little characteristic size particular importance.The various glue that consist of hydrocarbons can carry out etching in oxygen plasma,
Its reactional equation is
C
xH
y(Gu)+O
2(gas)+e
-→ CO (gas)+H
2O (gas).
In cavity, inject potassium hydroxide electrolyte and hole is shut back micro super capacitor preparation technology finish by liquid injection port.
Claims (7)
1. micro super capacitor that is applied to micro-system, it is characterized in that, the structure of described micro super capacitor is: go up preparation one deck thin nickel metal film collector (2) and ruthenium-oxide film (5) at silicon substrate (1), go up at ruthenium-oxide film (5) and to be supporting body structure between electrode (3 and liquid storage cavity fence structure (4), on supporting body structure between electrode (3), prepare ruthenium-oxide film (5) again, in liquid storage cavity fence structure (4), be liquid storage cavity between electrode (6) between supporter between electrode (3) and the ruthenium-oxide film (5), on whole micro super capacitor array, cover polyimides encapsulated layer (7) at last once more.
2. preparation method who is applied to the micro super capacitor of micro-system, it is characterized in that, the processing process of described micro super capacitor is: go up the figure of drawing out microcapacitor and array thereof by the method or the photoetching method of mask at silicon substrate (1), prepare one deck thin nickel metal film collector (2) and ruthenium-oxide film (5) then thereon as positive active material, spin coating one deck polyimide sacrificial layer once more on ruthenium-oxide film (5), by photoetching, developing procedure obtains supporting body structure (3) and liquid storage cavity fence structure (4) on every side, said structure is carried out the high-temperature sub amination treatment so that supporting body structure (3) and liquid storage cavity fence structure (4) obtain high structural strength and corrosion-resistant; Spin coating sacrifice layer and deposit ruthenium-oxide film (5) thereon successively once more after finishing imidization and handling as negative electrode active material layer, on negative electrode active material layer, get liquid injection hole, adopt the reactive plasma lithographic method that the polyimide sacrificial layer between both positive and negative polarity and oxygen reaction are formed carbon monoxide and these volatile substances of water then and finally discharge, form liquid storage cavity (6) between electrode, between the electrode that forms, pour into potassium hydroxide electrolyte then in the liquid storage cavity (6), and hole shut, on whole micro super capacitor array, cover polyimides rete (7) at last once more to finish encapsulation process.
3. according to claim 1 or the 2 described preparation methods that are applied to the micro super capacitor of micro-system, it is characterized in that described micro super capacitor adopts " liquid storage cavity between electrode " structure to replace traditional " electrode diaphragm stack " structure; This liquid storage cavity structure has been removed conventional membrane fully, setting by liquid storage cavity between microelectrode reaches the raising electrode activity, reduce the purpose of internal resistance between electrode, unique " liquid storage cavity structure between electrode " reduces micro element processing technology complexity greatly, be convenient to preparation in enormous quantities, effectively solve " electrode diaphragm laminated construction " intrinsic some technical barriers.
4. according to the described preparation method who is applied to the micro super capacitor of micro-system of claim 2, it is characterized in that the described graphics art of drawing out microcapacitor and array thereof is: preparation one deck SiO on silicon substrate
2Or spin coating one deck light-sensitive polyimide photoresist is as the sacrifice layer of metallic films such as preparation nickel, the figure of drawing out microcapacitor and array thereof by the method or the photoetching method of mask thereon.
5. according to the described preparation method who is applied to the micro super capacitor of micro-system of claim 2, it is characterized in that, the technology of preparing route of described nickel-base anode collector and ruthenium-oxide active material is: adopt evaporation, sputtering method to prepare one deck thin nickel metal film as collector on the figure of array, use the anodal layers of prepared ruthenium-oxide film such as vapour deposition CVD on the nickel collector.
6. according to the described preparation method who is applied to the micro super capacitor of micro-system of claim 2, it is characterized in that, the technology of preparing route of supporter and liquid storage cavity fence structure is between described positive and negative electrode: spin coating one deck polyimide sacrificial layer once more on the ruthenium-oxide active material layer, obtain needed supporting body structure and liquid storage cavity fence structure on every side by uv-exposure photoetching, developing procedure, supporting body structure is carried out the high-temperature sub amination treatment to obtain supporter and liquid storage cavity fence structure between high structural strength and corrosion resistant electrode.
7. according to the described preparation method who is applied to the micro super capacitor of micro-system of claim 2, it is characterized in that the technology of preparing route of described negative pole ruthenium-oxide active material and nickel collector is: spin coating sacrifice layer and adopt with anodal similarly method and deposit negative pole ruthenium-oxide active material layer and nickel film current collector layers thereon successively once more after finishing above-mentioned supporter and cavity structure and handling.
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Cited By (8)
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| CN101950686A (en) * | 2010-08-23 | 2011-01-19 | 清华大学 | Three-dimensional structure microelectrode applied to mini-super capacitor and manufacturing method thereof |
| CN102074371A (en) * | 2010-12-30 | 2011-05-25 | 清华大学 | Three-dimensional miniature super capacitor electrode manufactured from nano porous composite material and manufacturing method thereof |
| CN104701030A (en) * | 2015-03-24 | 2015-06-10 | 武汉理工大学 | All-solid-state symmetrical three-dimensional micro super capacitor and preparation method thereof |
| CN104766724A (en) * | 2015-03-06 | 2015-07-08 | 武汉理工大学 | Microfabrication process for micro capacitor based on cobaltosic oxide nano structure |
| CN104810163A (en) * | 2014-07-18 | 2015-07-29 | 纳米新能源（唐山）有限责任公司 | Graphene supercapacitor and preparation method thereof, and energy storage system |
| CN105869918A (en) * | 2016-04-06 | 2016-08-17 | 清华大学 | Carbon nanometer material based supercapacitor and fabrication method thereof |
| CN104377345B (en) * | 2013-08-15 | 2017-06-16 | 纳米新能源（唐山）有限责任公司 | Miniature energy storage device electrode, miniature energy storage device and forming method thereof |
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| FR2968824A1 (en) * | 2010-12-09 | 2012-06-15 | Centre Nat Rech Scient | Microcomponent e.g. micro-supercapacitor, for use in integrated system to store electricity, has electrodes formed on support surface and immersed in organic liquid electrolyte, where electrolyte is hermetically encapsulated within cavity |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101950686A (en) * | 2010-08-23 | 2011-01-19 | 清华大学 | Three-dimensional structure microelectrode applied to mini-super capacitor and manufacturing method thereof |
| CN101950686B (en) * | 2010-08-23 | 2012-02-08 | 清华大学 | Three-dimensional structure microelectrode applied to mini-super capacitor and manufacturing method thereof |
| CN102074371A (en) * | 2010-12-30 | 2011-05-25 | 清华大学 | Three-dimensional miniature super capacitor electrode manufactured from nano porous composite material and manufacturing method thereof |
| CN102074371B (en) * | 2010-12-30 | 2013-04-03 | 清华大学 | Three-dimensional miniature super capacitor electrode manufactured from nano porous composite material and manufacturing method thereof |
| CN104377345B (en) * | 2013-08-15 | 2017-06-16 | 纳米新能源（唐山）有限责任公司 | Miniature energy storage device electrode, miniature energy storage device and forming method thereof |
| CN104810163A (en) * | 2014-07-18 | 2015-07-29 | 纳米新能源（唐山）有限责任公司 | Graphene supercapacitor and preparation method thereof, and energy storage system |
| CN104810163B (en) * | 2014-07-18 | 2017-08-08 | 纳米新能源（唐山）有限责任公司 | Preparation method, graphene ultracapacitor and the energy-storage system of graphene ultracapacitor |
| CN104766724A (en) * | 2015-03-06 | 2015-07-08 | 武汉理工大学 | Microfabrication process for micro capacitor based on cobaltosic oxide nano structure |
| CN104766724B (en) * | 2015-03-06 | 2017-08-29 | 武汉理工大学 | A kind of button capacitor microfabrication based on cobaltosic oxide nano structure |
| CN104701030A (en) * | 2015-03-24 | 2015-06-10 | 武汉理工大学 | All-solid-state symmetrical three-dimensional micro super capacitor and preparation method thereof |
| CN104701030B (en) * | 2015-03-24 | 2017-09-29 | 武汉理工大学 | All solid state symmetric three-dimensional spiral micro super capacitor and preparation method thereof |
| CN105869918A (en) * | 2016-04-06 | 2016-08-17 | 清华大学 | Carbon nanometer material based supercapacitor and fabrication method thereof |
| CN105869918B (en) * | 2016-04-06 | 2018-07-06 | 江苏中天科技股份有限公司 | A kind of ultracapacitor based on carbon nanomaterial and preparation method thereof |
| CN113865160A (en) * | 2021-10-29 | 2021-12-31 | 势加透博（上海）能源科技有限公司 | Air circulation system |
| CN113865160B (en) * | 2021-10-29 | 2023-04-21 | 势加透博（上海）能源科技有限公司 | Air circulation system |
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