CN102751104A - Thick glue photoetching electroforming technology-based manufacture method of three-dimensional MEMS (micro-electromechanical systems) supercapacitor - Google Patents
Thick glue photoetching electroforming technology-based manufacture method of three-dimensional MEMS (micro-electromechanical systems) supercapacitor Download PDFInfo
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Abstract
The invention relates to a thick glue photoetching electroforming technology-based manufacture method of a three-dimensional MEMS (micro-electromechanical systems) supercapacitor. The supercapacitor has the structure of a comb tooth-shaped inserting finger. The method comprises the following steps of: on the substrate of a silicon wafer, taking SU-8 thick glue photoetching as a temperate, depositing a current collector in the template in an electroforming technology, electrically and chemically polymerizing a conducting polymer on the current collector to be taken as an active electrode material of the supercapacitor, and finally covering a layer of solid electrolyte. The supercapacitor has the three-dimensional structure, so that the superficial area of the electrode can be effectively enlarged, therefore, the energy density and the power density can be greatly improved relative to a flat plate structure. Furthermore, the safety performance of the method can be improved due to the use of solid electrolyte.
Description
Technical field
The present invention relates to a kind of MEMS ultracapacitor manufacturing approach based on the thick resist lithography electroforming process.
Background technology
Ultracapacitor (electrochemical capacitance) is a kind of novel energy-storing device between traditional capacitor and storage battery, has advantages such as power density is big, the time that discharges and recharges lacks, have extended cycle life, cryogenic property is good.The dual-use application of electrochemical capacitance is very extensive, little wireless senser to micron level, and the starting drive that arrives the rocket satellite greatly all be unable to do without electrochemical capacitance.Current research according to Lux shows that ultra-capacitor has huge market potential, 8.77 hundred million dollars of being expected to break through to 2014 from 2.08 hundred million dollars of 2008 of whole ultra-capacitor market income.
Small-sized electrochemical capacitance can be integrated because portable electric appts etc. with the IC circuit.The electrochemical capacitance integrated with the IC electric current can be used as stand-by power supply, when main power source is stopped power supply suddenly or during voltage collapse, ultracapacitor can start to memory, micro calculator, mainboard, these critical components power supplies such as clock; In addition, can provide pulse current that battery can not provide to satisfy high power requirements, make camera have continuous flash of light ability such as the electrochemical capacitance in the camera flash system with the integrated electrochemical capacitance of IC circuit; In addition, can be used as the storing apparatus of energy collecting system, can work up to a hundred hours after the solar energy wrist-watch with electrochemical capacitance is full of electricity by day, and this solar energy wrist-watch need not be changed electrochemical capacitance throughout one's life with the integrated electrochemical capacitance of IC circuit.Except aspect the consumer electronics, the electrochemical capacitance of miniaturization is because its high power density, and advantages such as long-life also have quite high using value aspect military or civilian wireless telecommunications and the wireless senser.
Electrochemical capacitance has application so widely and comes from advantages such as its power density is big, the time that discharges and recharges lacks, have extended cycle life, cryogenic property is good.The major defect of electrochemical capacitance be its energy density be merely lithium ion battery 5～7%.Therefore, how to improve the performance of electrochemical capacitance, especially energy density becomes the major subjects that electrochemical capacitance is studied.
As a rule, according to charge-storage mechanism, ultra-capacitor can be divided into two kinds of electric double layer capacitance and electrochemical capacitors.The electric capacity of electric double layer derives from the electrostatic attraction (similar traditional capacitor) of physics, and the capacity of electrochemical capacitor is from redox reaction (similar battery).The capacity density of every type electrochemical capacitance all with the effective area positive correlation of electrode material, therefore to improve the research of performance of electrochemical capacitance very extensive about introducing nanometer technology, especially improves the performance of electrochemical capacitance through the preparation nano-electrode material.Wherein CNT is maximum as the electrode material research of electric double layer capacitance; Metal nanoparticle also can be used as the electrode of electrochemical capacitance; The typical electrode materials conducting polymer of electrochemistry electrochemical capacitance also is made into nanostructure and is studied; Metal oxide has also improved performance through nano modification as the material of another electrochemistry electrochemical capacitance, and researchers have also prepared the carbon nano tube/conducting polymer compound film electrode in addition, attempts to bring into play the double action of electric double layer capacitance and electrochemical capacitor.
Yet; Electrode material only is a key component of electrochemical capacitance system, how according to electrode material select suitable electrochemical capacitance system (comprising electrochemical capacitance structure, electrolyte, collector etc.), preparation processing method and with integrated (comprising the integrated of the integrated of small size chip-scale and large scale hybrid energy system) of circuit also be the especially major issue used of electrochemical capacitance of research electrochemical capacitance.Increasingly mature MEMS (MEMS) technology provides good condition for the chip-scale of electrochemical capacitance and other function elements is integrated.Yet now to the integrated electrochemical capacitance of chip of silicon chip level technology or to be integrated in the electrochemical capacitance research of printed circuit board (PCB) very limited.Korea S Sung has prepared all solid state electrochemical capacitance of plane comb structure based on silicon base, yet because structure is too simple, does not effectively carry out space utilization and cause this electrochemical capacitance performance not high.Y.Q.Jiang has prepared the electrode of the high CNT forest of 80 μ m as electrochemical capacitance on silicon chip, obtained 428 μ F cm
-2Specific capacity and 0.28 mW cm
-2The electric double layer electrochemical capacitance of specific power, its energy density is still limited, and liquid electrolyte has increased its integrated difficulty and the occasion that has limited its application in addition.For the problem of electrochemical capacitance and the integrated aspect of plated circuit, once had two Americans to study the circuit board integral printing of ultra-capacitor, but technical data that has no and scientific and technical literature are published.
Summary of the invention
The present invention proposes a kind of novel three-dimensional MEMS electrochemical capacitance, and this electrochemical capacitance utilizes the manufacturing of MEMS processing method to form.Adopt the MEMS processing technology of existing maturation; On silicon or substrate of glass; Utilize micro-nano technology to process the very large three-dimensional structure of specific area, combined with electrochemical conducting polymer electrode preparation technology realizes high power density, high-energy-density and long cycle lie.All processing process of the present invention and printed circuit board (PCB) or other MEMS device fabrications are compatible, therefore both can form hybrid energy system with energy harvester or micro cell, can embed electronic circuit system again and be applied to consumer electronics and wireless device.
The technical scheme that the present invention adopts is:
May further comprise the steps based on thick resist lithography electroforming process three-dimensional MEMS ultracapacitor manufacturing approach:
(1) silicon chip cleans, and cleaning step is for being followed successively by organic oil removing, and inorganic oil removing is removed oxide-film and removed metal ion.
(2) put cleaned silicon chip in the step (1) into oxidation furnace and carry out thermal oxidation, the oxide-film of formation is as the electric insulation layer of two electrodes of ultracapacitor.
(3) put well-oxygenated silicon chip in the step (2) into vacuum sputter system sputter electroforming Seed Layer.
(4) in step (3), have the method that adopts rotation to spare glue on the silicon chip of electroforming Seed Layer and be coated with the last layer thick photoresist, exposure is developed, and solidifies the three-dimensional broach template of back formation.
(5) silicon chip that has the three-dimensional broach template of thick glue in the step (4) is put into carried out electroforming in the electroplating pool until filling full whole broach template; Remove the Seed Layer below thick glue pattern plate and the template with the method for chemical corrosion then, insert the collector that refers to structure thereby on silicon chip, form to have.
(6) put into and carry out electrochemical polymerization in the electrochemical reaction cell having the silicon chip that insert to refer to the structure collector in the step (5), form the conducting polymer electrode at collection liquid surface.
(7) in step (6), have and apply one deck solid electrolyte on the silicon chip of conducting polymer electrode and form three-dimensional MEMS ultracapacitor device.
Cleaning is a silicon chip standard cleaning technology in the said step (1).
Thermal oxidation is a means of wet thermal oxidation in the said step (2), and thickness is the 0.5-1.5 micron.
Electroforming Seed Layer in the said step (3) is a kind of of gold, platinum, nickel, and thickness is the 100-500 nanometer.
Photoresist in the said step (4) can be negative glue SU-8 or positive glue PMMA (polymethyl methacrylate), and the three-dimensional structure width is the 5-200 micron, and thickness is the 100-1000 micron, and curing temperature is 80-100 degree centigrade.
The removal method of the photoresist template in the said step (4) is chemical corrosion.
Collector in the said step (5) is a kind of of gold, copper or nickel, and the electroforming current density is 10-50 mAcm
-2, temperature is 30-90 degree centigrade.
Conducting polymer in the said step (6) is a polypyrrole, polyaniline, and one or both of polythiophene or its derivative also can be composite conductive high molecular.
Electrochemical polymerization solution in the said step (6) contains large-scale anion, and current density is 0.1-10 mAcm
-2
Solid electrolyte in the said step (7) is a gel state electrolyte, contains the less relatively anion of size.
Advantage of the present invention is: used technology is compatible mutually with ripe MEMS technology in the entire device course of processing; Three-dimensional micro-electrode structure of the present invention effectively raises the effective surface area of unit area basis area, thereby improves the specific energy and the specific power of ultracapacitor device.In addition, the application of solid electrolyte has improved the security performance of ultracapacitor.
Description of drawings
Fig. 1 is the structural representation of ultracapacitor instance of the present invention; SiO among the figure
2/ Si Substrate is SiO
2/ Si substrate; Solid state electrolyte is a solid electrolyte; Output is output;
Fig. 2 is the processing process figure of instance of the present invention.
Embodiment
The structural representation of ultracapacitor instance of the present invention is as shown in Figure 1.
As shown in Figure 2, based on thick resist lithography electroforming process three-dimensional MEMS ultracapacitor manufacturing approach, may further comprise the steps:
(1) choose 4 cun silicon chips as substrate, silicon chip cleans in xylenes, acetone, alcohol, sulfuric acid/hydrogen peroxide solution, ammoniacal liquor/hydrogen peroxide solution, hydrochloric acid/hydrogen peroxide solution to remove greasy dirt, oxide-film and metal ion successively.
(2) put cleaned silicon chip in the step (1) into oxidation furnace and carried out means of wet thermal oxidation 10 hours, oxidated layer thickness is 1.5 microns.
(3) in step (2) on the well-oxygenated silicon chip rf magnetron sputtering one layer thickness be that the nickel of 300 nanometers is as the electroforming Seed Layer.
(4) method that adopts rotation to spare glue on the nickel dam in step (3) is coated with the SU-8 photoresist of last layer Microchem company; Before 95 degrees centigrade, dried by the fire 4 hours after leaving standstill bubble collapse; Made public 320 seconds; Developed 4 hours, formation thickness is 450 microns three-dimensional comb structure after baking is solidified 4 hours after 95 degrees centigrade.
(5) with the three-dimensional comb structure in the step (4) as template, carry out the collector of electroformed nickel above that as ultracapacitor, current density is 20mAcm
-2, the electroforming time is about 20 hours, the watt electroplate liquid of electroforming solution for improveing.When the thickness of electroformed nickel reaches template thickness, stop electroforming, erode the Seed Layer below template and the template, insert the nickel collector that refers to structure thereby on silicon chip, form to have.
(6) in step (5), in electrolytic cell, carry out polypyrrole (PPy) electrochemical polymerization on the nickel collector, electrolyte ph is 4 and contains the mix ion of p-methyl benzenesulfonic acid anion as polypyrrole that the polymerization current density is 1 mAcm
-2, polymerization temperature is 25 degrees centigrade, polymerization time is 30 minutes.
(7) POLYPROPYLENE GLYCOL/lithium perchlorate/water that on step (6) polypyrrole electrode, applies the layer of gel attitude is accomplished the encapsulation of whole three-dimensional MEMS ultracapacitor as the solid electrolyte of this ultracapacitor.
The three-dimensional MEMS ultracapacitor of as above being processed is tested on electrochemical workstation, at 5 mAcm
-2Recording its specific capacity under the discharge rate is 0.029 Fcm
-2
The present invention has improved the surface area of electrode of super capacitor through micro fabrication, thereby has improved the energy density and the power density of ultracapacitor.All processing technologys among the present invention and other MEMS devices for example processing technology of pressure sensor, energy harvester etc. are compatible mutually, but therefore have very high integration, have in fields such as microelectronics, transducers widely and use.
Claims (8)
1. based on the three-dimensional MEMS ultracapacitor manufacturing approach of thick resist lithography electroforming process, it is characterized in that, may further comprise the steps:
(1) silicon chip cleans, and cleaning step is for being followed successively by organic oil removing, and inorganic oil removing is removed oxide-film and removed metal ion;
(2) put cleaned silicon chip in the step (1) into oxidation furnace and carry out thermal oxidation, the oxide-film of formation is as the electric insulation layer of two electrodes of ultracapacitor;
(3) put well-oxygenated silicon chip in the step (2) into vacuum sputter system sputter electroforming Seed Layer;
(4) in step (3), have the method that adopts rotation to spare glue on the silicon chip of electroforming Seed Layer and be coated with the last layer thick photoresist, exposure is developed, and solidifies the three-dimensional broach template of back formation;
(5) silicon chip that has the three-dimensional broach template of thick glue in the step (4) is put into carried out electroforming in the electroplating pool until filling full whole broach template; Remove the Seed Layer below thick glue pattern plate and the template with chemical method then, insert the collector that refers to structure thereby on silicon chip, form to have;
(6) put into and carry out electrochemical polymerization in the electrochemical reaction cell having the silicon chip that insert to refer to the structure collector in the step (5), form the conducting polymer electrode at collection liquid surface;
(7) in step (6), have and apply one deck solid electrolyte on the silicon chip of conducting polymer electrode and form three-dimensional MEMS ultracapacitor device.
2. the three-dimensional MEMS ultracapacitor manufacturing approach based on the thick resist lithography electroforming process according to claim 1 is characterized in that, the electroforming Seed Layer is a kind of of metallic gold, platinum or nickel in the said step (3), and thickness is the 100-500 nanometer.
3. the three-dimensional MEMS ultracapacitor manufacturing approach based on the thick resist lithography electroforming process according to claim 1; It is characterized in that; Photoresist in the said step (4) can be negative glue SU-8 or positive glue polymetylmethacrylate; The three-dimensional structure width is the 5-200 micron, and thickness is the 100-1000 micron, and curing temperature is 80-100 degree centigrade.
4. the three-dimensional MEMS ultracapacitor manufacturing approach based on the thick resist lithography electroforming process according to claim 1 is characterized in that the removal method of the photoresist template in the said step (4) is chemical corrosion.
5. the three-dimensional MEMS ultracapacitor manufacturing approach based on the thick resist lithography electroforming process according to claim 1 is characterized in that, the collector in the said step (5) is a kind of of gold, copper or nickel, and the electroforming current density is 10-50 mAcm
-2, temperature is 30-90 degree centigrade.
6. the three-dimensional MEMS ultracapacitor manufacturing approach based on the thick resist lithography electroforming process according to claim 1; It is characterized in that the conducting polymer in the said step (6) is a polypyrrole, polyaniline; One or both of polythiophene or its derivative also can be composite conductive high molecular.
7. the three-dimensional MEMS ultracapacitor manufacturing approach based on the thick resist lithography electroforming process according to claim 1 is characterized in that the electrochemical polymerization solution in the said step (6) contains large-scale anion, and current density is 0.1-10 mAcm
-2
8. the three-dimensional MEMS ultracapacitor manufacturing approach based on the thick resist lithography electroforming process according to claim 1 is characterized in that the solid electrolyte in the said step (7) is a gel state electrolyte, contains the less relatively anion of size.
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| CN104465125A (en) * | 2014-11-28 | 2015-03-25 | 太原理工大学 | TiO2/NiO three-dimensional inter-digital microelectrode and preparing method thereof |
| CN104599864A (en) * | 2015-01-22 | 2015-05-06 | 太原理工大学 | Oblique photoetching method capable of increasing specific surface area of MEMS super-capacitor electrode |
| CN104681304A (en) * | 2015-03-20 | 2015-06-03 | 太原理工大学 | Preparation method of asymmetric supercapacitor |
| 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 |
| 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 |
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| CN111063548A (en) * | 2019-12-13 | 2020-04-24 | 江苏大学 | Three-dimensional silicon structure/polyaniline-based composite electrode material and preparation method thereof |
| CN112382511A (en) * | 2020-10-14 | 2021-02-19 | 北京理工大学 | Self-charging micro optical capacitor device and preparation method thereof |
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| 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 |
| CN104465125B (en) * | 2014-11-28 | 2017-12-01 | 太原理工大学 | TiO2Three-dimensional interdigital microelectrodes of/NiO and preparation method thereof |
| CN104465125A (en) * | 2014-11-28 | 2015-03-25 | 太原理工大学 | TiO2/NiO three-dimensional inter-digital microelectrode and preparing method thereof |
| CN104599864A (en) * | 2015-01-22 | 2015-05-06 | 太原理工大学 | Oblique photoetching method capable of increasing specific surface area of MEMS super-capacitor electrode |
| CN104681304A (en) * | 2015-03-20 | 2015-06-03 | 太原理工大学 | Preparation method of asymmetric supercapacitor |
| CN104681304B (en) * | 2015-03-20 | 2017-08-25 | 太原理工大学 | A kind of Asymmetric Supercapacitor preparation method |
| 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 |
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| CN109659153A (en) * | 2018-12-18 | 2019-04-19 | 清华大学 | A kind of metal oxide and the compound micro comb energy storage electrode of carbon nanotube |
| CN109809359A (en) * | 2019-01-10 | 2019-05-28 | 北方工业大学 | 2.5D interdigital electrode manufacturing method and interdigital electrode |
| CN111063548A (en) * | 2019-12-13 | 2020-04-24 | 江苏大学 | Three-dimensional silicon structure/polyaniline-based composite electrode material and preparation method thereof |
| CN112382511A (en) * | 2020-10-14 | 2021-02-19 | 北京理工大学 | Self-charging micro optical capacitor device and preparation method thereof |
| CN112382511B (en) * | 2020-10-14 | 2021-08-13 | 北京理工大学 | Self-charging micro optical capacitor device and preparation method thereof |
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