CN104217863B - Field-effect regulates and controls the preparation method of ultracapacitor - Google Patents
Field-effect regulates and controls the preparation method of ultracapacitor Download PDFInfo
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- CN104217863B CN104217863B CN201410458341.3A CN201410458341A CN104217863B CN 104217863 B CN104217863 B CN 104217863B CN 201410458341 A CN201410458341 A CN 201410458341A CN 104217863 B CN104217863 B CN 104217863B
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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
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Abstract
The invention discloses the preparation method that a kind of field-effect regulates and controls ultracapacitor.Its process is as follows：One dielectric layer material is deposited on substrate；Electrode material is dispersed in described dielectric layer material；The painting erosion resistant agent on dielectric layer and raceway groove, prepares an electrode of source electrode, drain electrode and capacitor；The coating photoresist in source electrode, drain electrode；Dimethyl silicone polymer overall package is used, electrolyte is injected, field-effect regulation and control ultracapacitor is obtained.Propose a kind of thinking for improving super capacitor energy density, the Carrier Profile for changing material itself by additional field-effect is optimized with electric conductivity to energy storage device, under the regulating and controlling effect of gate electric field, the capacity of ultracapacitor averagely has 3 to 5 times of lifting, and maintains original high rate performance.
Description
Technical field
The invention belongs to capacitor technology field, and in particular to a kind of field-effect regulates and controls the preparation method of ultracapacitor.
Background technology
Ultracapacitor, is grow up the seventies and eighties in 20th century a kind of between battery and traditional capacitor
New type of energy storage device, the super large capacitor amount with farad level, the electrolytic capacitor capacity than same volume is big 2000-6000 times, work(
Rate density ratio battery is high 10-100 times, while having longer cycle life, it is considered to be a kind of Novel clean efficiently, practical
The energy, currently as stand-by power supply, is widely used in the electronic device product such as camera, video recorder, mobile phone, computer
In.
Ultracapacitor can be divided into electric double layer capacitance and fake capacitance according to the difference of energy storage mechnism.The product of electric double layer capacitance
Life is based primarily upon the electric double layer capacitance on electrode/electrolyte interface produced by separation of charge, such as carbon electrode capacitor；Pseudocapacitors
The generation of electric capacity is that underpotential deposition occurs on noble metal electrode surface based on electroactive ion, or in noble metal oxide electrodes
The adsorption capacitance that surface occurs redox reaction and produces.
In existing research, either electric double layer capacitance or fake capacitance, the effective ways for improving condenser capacity are all carried
The specific surface area of high electrode material.Double layer capacitor is generally using the activated carbon of high-specific surface area；Pseudocapacitors are generally used
The metal oxide of nano particle size.But, the micropore surface that can be only contacted with electrolyte in electrode material could produce electricity
Hold, the deficiency of existing double layer capacitor and pseudocapacitors is that the major part of porous electrode surface area is micropore, due to
The effect of electrolyte solution surface tension, makes electrolyte solution be difficult to enter into the micropore of porous electrode, causes electrode material
Surface area utilization rate is low, or even the carbon electrode material specific surface area having is very big, but electric capacity is little after being made capacitor
Phenomenon.
For improving the low density problem of capacitor energy, now common thinking has two aspects, and one is：By changing material
The contact area of the dimensional structure of material, increase material and electrolyte.Such as scantling nanosizing, or prepare porous knot
Structure；Two are：By compound with other materials, chemically improve its energy-storage property, such as MnO on composition2It is compound with Graphene.
Above ameliorative way preparation technology is complicated, and cost of manufacture is higher, and method universality is poor.
The content of the invention
Present invention aim at a kind of method for increasing capacity of super capacitor of offer.
It is as follows using technical scheme to reach above-mentioned purpose：
A kind of field-effect regulates and controls the preparation method of ultracapacitor, comprises the following steps：
The raceway groove of field-effect transistor is prepared to electrode as the electrode material of ultracapacitor, and coating photoresist is covered
Source, the drain electrode of field-effect transistor are covered, electrolyte is encapsulated.
By such scheme, the material that the raceway groove is used is electrode material.
A kind of field-effect regulates and controls the preparation method of ultracapacitor, comprises the following steps
One dielectric layer material is deposited on substrate；Electrode material is dispersed in described dielectric layer material；In dielectric
Painting erosion resistant agent on layer and raceway groove, prepares an electrode of source electrode, drain electrode and capacitor；Photoetching is coated with source electrode, drain electrode
Glue；Dimethyl silicone polymer overall package is used, electrolyte is injected, field-effect regulation and control ultracapacitor is obtained.
Beneficial effects of the present invention：
A kind of thinking for improving super capacitor energy density is proposed, i.e., material itself is changed by additional field-effect
Carrier Profile is optimized with electric conductivity to energy storage device, meanwhile, for we are right the characteristics of electric field strength can easily be accommodated
Real-time monitoring is carried out there is provided feasibility in capacity of super capacitor；
Under the regulating and controlling effect of gate electric field, the capacity of ultracapacitor averagely has 3 to 5 times of lifting, and maintains original
Some high rate performances.
Brief description of the drawings
Fig. 1：:The field-effect regulation and control ultracapacitor cyclic voltammetry curve figure of embodiment 1；
Fig. 2：:The field-effect regulation and control ultracapacitor high rate performance figure of embodiment 1；
Fig. 3：:The field-effect regulation and control ultracapacitor cyclic voltammetry curve figure of embodiment 2.
Specific embodiment
Detailed description below further explains technical scheme, but not as to the scope of the present invention
Limitation.
Field-effect of the present invention regulates and controls the preparation process of ultracapacitor：
One dielectric layer material is deposited on substrate；Electrode material is dispersed in described dielectric layer material；In dielectric
Painting erosion resistant agent on layer and raceway groove, prepares an electrode of source electrode, drain electrode and capacitor；Photoetching is coated with source electrode, drain electrode
Glue；Dimethyl silicone polymer overall package is used, electrolyte is injected, field-effect regulation and control ultracapacitor is obtained.
The Carrier Profile for changing material itself by additional field-effect is optimized with electric conductivity to energy storage device, in grid
Under the regulating and controlling effect of pole electric field, the capacity of ultracapacitor averagely has 3 to 5 times of lifting, and maintains original high rate performance.
Embodiment 1
1) from the silicon chip with 300nm thermal oxide layers, silicon chip is cut into appropriate size, then uses isopropanol
(IPA) it is cleaned by ultrasonic silicon chip about 30s, is dried up with nitrogen.
2) spin coating instrument one layer of MMA of spin coating on substrate is used, the rotating speed of spin coating is 4000rpm, and spin-coating time is 90s, is made
Toasted with electric hot plate, 180 DEG C, 5min；Then one layer of PMMA of spin coating on substrate again, the rotating speed of spin coating is 4000rpm, during spin coating
Between be 90s, toasted using electric hot plate, 180 DEG C, 5min.
3) pattern of external electrode and mark is etched on the good silicon chip of spin coating using electron beam exposure apparatus (EBL), agent is exposed
It is 380 μ C/cm to measure2, beam voltage is 30kV, and electron beam current is 400pA.
4) develop：Substrate after electron beam exposure is soaked into 1min in methylisobutylketone (MIBK) solution, then different
30s, nitrogen drying are soaked in propyl alcohol.
5) Plasma cleanings：Use O2Plasma cleaning silicon chips, power is 50W, clean 5min, O2 flows 30-60mL/
min。
6) metal thermal evaporation (PVD)：Metal external electrode and mark, Cr/Au (5nm/50nm) are steamed using thermal evaporation plated film instrument.
7) metal-stripping：The substrate that will be deposited with has metal is put and stands 12h in acetone, MMA/PMMA is all peeled off, so
Acetone and isopropanol rinse substrate, nitrogen drying are used afterwards.
8) by MnO2Nano wire is dispersed on substrate：The MnO that will synthesize2Nano wire is dispersed in absolute ethyl alcohol by ultrasonic machine
In, then it is dispersed on substrate by spin coating instrument, position and concentration of the nano wire on substrate are appropriate.
9) sample is taken pictures under an optical microscope, is drawn using NPGS, marking nano line is specific on substrate
The interior electrode pattern of position, design connection nano wire and external electrode.
10) spin coating instrument one layer of MMA of spin coating on substrate is used, the rotating speed of spin coating is 4000rpm, and spin-coating time is 90s, is made
Toasted with electric hot plate, 180 DEG C, 5min.Then one layer of PMMA of spin coating on substrate again, the rotating speed of spin coating is 4000rpm, during spin coating
Between be 90s, toasted using electric hot plate, 180 DEG C, 5min.
11) interior electrode pattern is etched using electron beam exposure apparatus (EBL), exposure dose is 380 μ C/cm2, electronics accelerate (beamacceleration)
Voltage is 30kV, and electron beam current is 100pA.
12) develop：Substrate after electron beam exposure is soaked into 1.5min, Ran Hou in methylisobutylketone (MIBK) solution
30s, nitrogen drying are soaked in isopropanol.
13) metal thermal evaporation (PVD)：Metal inner electrode, Cr/Au (5nm/150nm) are steamed using thermal evaporation plated film instrument.
14) metal-stripping：The substrate that will be deposited with has metal is put and stands 12h in acetone, MMA/PMMA is all peeled off, so
Acetone and isopropanol rinse substrate, nitrogen drying are used afterwards.
15) spin coating instrument one layer of SU82002 of spin coating on substrate is used, the rotating speed of spin coating is 4000rpm.Dried using electric hot plate
It is roasting SU8,65 DEG C, 5min；95℃,5min.
16) SU8 patterns are made using electron beam exposure apparatus, SU8 is just covered and protect metal electrode, prevented in solution
Metal electrode and solution are contacted during middle electrical testing.Exposure dose is 3 μ C/cm2, beam voltage is 30kV, electron beam
Electric current is 20pA.
17) baking after being exposed to SU8,65 DEG C, 1min；95 DEG C, 1min.
18) develop：Substrate is placed on SU8 developer immersion 1min respectively, 30s, nitrogen are then soaked in isopropanol
Air-blowing is done.
19) rigid baking treatment is carried out to SU8：Place the substrates on electric hot plate, electric hot plate is from room temperature to 180
DEG C, 60min is incubated at 180 DEG C, electric hot plate is naturally cooled to room temperature.
20) dimethyl silicone polymer (PDMS) packaging is utilized, by microflow control technique, electrolysis is prepared in glove box
Liquid KOH (6M) simultaneously injects electrolyte by guiding tube, obtains field-effect regulation and control ultracapacitor.
Field-effect manufactured in the present embodiment regulates and controls ultracapacitor cyclic voltammetry curve figure, referring to the drawings 1.In back gate voltage
When respectively 1 V, 2 V, 3 V and 4 V, MnO2Single nanometer energy storage device is in the case where 30mV/s sweeps speed as shown in figure 1, back gate voltage
During for 3 V, condenser capacity obtains 2.5 times of lifting.
Field-effect manufactured in the present embodiment regulates and controls ultracapacitor high rate performance figure, referring to the drawings 2.Nano-device is with the back of the body
The increase of gate voltage, MnO2Its high rate performance is not decayed while the capacity of single nanometer energy storage device is improved significantly.
Embodiment 2
Field-effect regulates and controls the preparation process of ultracapacitor nano-device：
It is the Al of 80nm using ALD deposition thickness from silicon chip2O3, as dielectric layer.
Using spin coating instrument on substrate one layer of MMA of spin coating, the rotating speed of spin coating is 4000rpm, and spin-coating time is 90s, is used
Electric hot plate is toasted, 180 DEG C, 5min；Then one layer of PMMA of spin coating on substrate again, the rotating speed of spin coating is 4000rpm, spin-coating time
It is 90s, is toasted using electric hot plate, 180 DEG C, 5min.
The pattern of external electrode and mark, exposure dose are etched on the good silicon chip of spin coating using electron beam exposure apparatus (EBL)
It is 380 μ C/cm2, beam voltage is 30kV, and electron beam current is 400pA.
Development：Substrate after electron beam exposure is soaked into 1min in methylisobutylketone (MIBK) solution, then in isopropyl
30s, nitrogen drying are soaked in alcohol.
Plasma is cleaned：Use O2Plasma cleaning silicon chips, power is 50W, clean 5min, O2 flows 30-60mL/
min。
Metal thermal evaporation (PVD)：Metal external electrode and mark, Cr/Au (5nm/50nm) are steamed using thermal evaporation plated film instrument.
Metal-stripping：The substrate that will be deposited with has metal is put and stands 12h in acetone, MMA/PMMA is all peeled off, then
With acetone and isopropanol rinse substrate, nitrogen drying.
By the dispersion of MoS2 nanometer sheets on the dielectric layer.
Sample is taken pictures under an optical microscope, is drawn using NPGS, specific position of the marking nano line on substrate
Put, the interior electrode pattern of design connection nano wire and external electrode.
Using spin coating instrument on substrate one layer of MMA of spin coating, the rotating speed of spin coating is 4000rpm, and spin-coating time is 90s, is used
Electric hot plate is toasted, 180 DEG C, 5min.Then one layer of PMMA of spin coating on substrate again, the rotating speed of spin coating is 4000rpm, spin-coating time
It is 90s, is toasted using electric hot plate, 180 DEG C, 5min.
Interior electrode pattern is etched using electron beam exposure apparatus (EBL), exposure dose is 380 μ C/cm2, electronics accelerate (beamacceleration) electricity
It is 30kV to press, and electron beam current is 100pA.
Development：Substrate after electron beam exposure is soaked into 1.5min in methylisobutylketone (MIBK) solution, then different
30s, nitrogen drying are soaked in propyl alcohol.
Metal thermal evaporation (PVD)：Metal inner electrode, Cr/Au (5nm/150nm) are steamed using thermal evaporation plated film instrument.
Metal-stripping：The substrate that will be deposited with has metal is put and stands 12h in acetone, MMA/PMMA is all peeled off, then
With acetone and isopropanol rinse substrate, nitrogen drying.
Using spin coating instrument on substrate one layer of SU8 2002 of spin coating, the rotating speed of spin coating is 4000rpm.Toasted using electric hot plate
SU8,65℃,5min；95℃,5min.
SU8 patterns are made using electron beam exposure apparatus, SU8 is just covered and is protected metal electrode, prevented in the solution
Metal electrode and solution are contacted during electrical testing.Exposure dose is 3 μ C/cm2, beam voltage is 30kV, electron beam electricity
It is 20pA to flow.
Baking after being exposed to SU8,65 DEG C, 1min；95 DEG C, 1min.
Development：Substrate is placed on SU8 developer immersion 1min respectively, 30s is then soaked in isopropanol, nitrogen blows
It is dry.
Rigid baking treatment is carried out to SU8：Place the substrates on electric hot plate, electric hot plate from room temperature to 180 DEG C,
180 DEG C of insulation 60min, then make electric hot plate naturally cool to room temperature.
Using dimethyl silicone polymer (PDMS) packaging, by microflow control technique, electrolyte is prepared in glove box
And electrolyte is injected by guiding tube, obtain the ultracapacitor of field-effect regulation and control.
Field-effect manufactured in the present embodiment regulates and controls ultracapacitor cyclic voltammetry curve figure, referring to the drawings 3.Back gate voltage exists
During 0-2.5 V, 100mV/s sweeps the cyclic voltammetry curve figure under speed, as shown in figure 3, its capacity has obtained 5 times of raising.
Claims (1)
1. a kind of field-effect regulates and controls the preparation method of ultracapacitor, it is characterised in that comprise the following steps：
One dielectric layer material is deposited on substrate；Electrode material is dispersed in described dielectric layer material；In dielectric layer and
Painting erosion resistant agent on raceway groove, prepares an electrode of source electrode, drain electrode and capacitor；The coating photoresist in source electrode, drain electrode；With
Dimethyl silicone polymer overall package, injects electrolyte, obtains field-effect regulation and control ultracapacitor.
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| CN201410458341.3A CN104217863B (en) | 2014-09-10 | 2014-09-10 | Field-effect regulates and controls the preparation method of ultracapacitor |
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| CN104730125B (en) * | 2015-03-20 | 2017-10-24 | 武汉理工大学 | A kind of in-situ study Li+Ion or Na+The method of ion discharge and recharge transport mechanism in nano wire |
| CN105470001A (en) * | 2015-12-08 | 2016-04-06 | 武汉理工大学 | MoS2 nanosheet dual-gate field effect transistor/supercapacitor composite device and manufacturing method therefor |
| KR102018309B1 (en) * | 2017-10-31 | 2019-09-04 | 삼성전기주식회사 | Capacitor Component And Manufacturing Method Of The Same |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1052006A (en) * | 1989-11-20 | 1991-06-05 | 三星电子株式会社 | Semiconductor device and manufacture method thereof |
| CN1871675A (en) * | 2003-08-20 | 2006-11-29 | 波尔伊克两合公司 | Organic capacitor having a voltage-controlled capacitance |
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| JP2007273797A (en) * | 2006-03-31 | 2007-10-18 | Central Res Inst Of Electric Power Ind | Electrode for capacitor and electric double layer capacitor using same |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1052006A (en) * | 1989-11-20 | 1991-06-05 | 三星电子株式会社 | Semiconductor device and manufacture method thereof |
| CN1871675A (en) * | 2003-08-20 | 2006-11-29 | 波尔伊克两合公司 | Organic capacitor having a voltage-controlled capacitance |
Non-Patent Citations (1)
| Title |
|---|
| New opportunities for organic electronics and bioelectronics: ions in action;Giuseppe Tarabella等;《Chemical Science》;20121206;第4卷;第1395-1409页 * |
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