CN109216035A - A kind of all solid state plane asymmetric miniature ultracapacitor device and preparation method thereof - Google Patents
A kind of all solid state plane asymmetric miniature ultracapacitor device and preparation method thereof Download PDFInfo
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- CN109216035A CN109216035A CN201711319977.XA CN201711319977A CN109216035A CN 109216035 A CN109216035 A CN 109216035A CN 201711319977 A CN201711319977 A CN 201711319977A CN 109216035 A CN109216035 A CN 109216035A
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- solid state
- plane asymmetric
- ultracapacitor device
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/04—Hybrid capacitors
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
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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 present invention relates to micro-nano device manufacturing field, specially a kind of all solid state plane asymmetric miniature ultracapacitor device and preparation method thereof.The all solid state plane asymmetric miniature ultracapacitor device mainly includes following sections: flexible substrates, the nonmetallic collector of the patterning being deposited in substrate and electrode material, solid-state electrolytic solution.The beneficial effects of the present invention are: not only having remained the advantage of the high power density of supercapacitor using high capacitance electrode material, but also the operating voltage of supercapacitor is improved, and then improve energy density.The technology have the advantages that simple process, processing cost it is low, it is high-efficient, can be mass-produced, the micro-nano devices such as MEMS, microrobot, implantable medical device field can be widely used in, laid a good foundation for the development of micro-nano electronic equipment.
Description
Technical field:
The invention belongs to micro-nano device manufacturing field, specially a kind of all solid state plane asymmetric miniature ultracapacitor device and
Preparation method.
Background technique:
The fast development of miniaturized electronic devices (such as MEMS, microrobot, miniature implantable medical device)
It greatly have stimulated the urgent need to miniature power source.Planar miniature supercapacitor due to power density with higher,
Energy density, excellent cycle performance are increasingly becoming a kind of emerging chip energy storage device.To further increase microdevice
Energy density, research and development plane asymmetric miniature ultracapacitor device are an effective new ways.Currently, non-about plane
In the system of symmetrical button capacitor electrode material, since its positive and negative pole material does not match preferably, electrode utilization rate is not high,
Cause the coulombic efficiency of corresponding device not high, energy density is lower, and preparation method is complicated.Therefore, it matches and establishes one newly
Asymmetric electrode material system, it is asymmetric micro- to find a kind of low cost, high efficiency, easily operated, precisely controllable plane
The magnanimity technology of preparing of type supercapacitor has important strategy for plane asymmetric miniature ultracapacitor device practical application
Meaning.
Summary of the invention:
It is asymmetric miniature super it is an object of the invention to develop a kind of high power density, all solid state plane of high-energy density
Grade capacitor provides a kind of inexpensive, high-efficient, easily operated, mask plate aided filter method that controllability is good to prepare plane
Asymmetric miniature ultracapacitor device.
In order to achieve the above object, the technical solution of the present invention is as follows: a kind of all solid state plane asymmetric miniature ultracapacitor
Device mainly includes following sections: flexible substrates, the nonmetallic collector of the patterning being deposited in substrate and electrode material, Gu
State electrolyte.It is characterized in that the both ends of the patterned electrodes load different anode and negative electrode material respectively.This is entirely solid
The preparation method of state plane asymmetric miniature ultracapacitor device is mask plate aided filter method, it is characterised in that described is nonmetallic
Collector and positive and negative electrode material are to be filtered respectively using filtering technique at the both ends of pattern mask plate.
According to above scheme, the flexible substrates that the present invention uses include various filter paper (cellulose mixture film, nylon membrane etc.),
PET, polyethylene diagrams, polypropylene diaphragm, paper, textile material, preferably cellulose mixture film, nylon membrane, PET.
According to above scheme, nonmetallic collector that the present invention uses is good conductivity, smooth material, as graphene,
Carbon nanotube, PH1000, with a thickness of 10nm-10 μm, preferably 100nm-2 μm of
According to above scheme, the configuration for the patterned electrodes that the present invention uses includes level-crossing finger-type, concentric ring type, puts down
Line type, parallel fold lines type, concentric interdigital, having a size of 10 μm of -10cm, preferred size is 100 μm of -1cm；With a thickness of
100nm-200 μm, preferred thickness is 200nm-10 μm.
According to above scheme, the present invention make in positive electrode include graphene, active carbon, carbon nanotube, Co (OH)2、
Ni(OH)2、Co3O4、MnO2, negative electrode material includes graphene, active carbon, carbon nanotube, VN, TiN, Mn3O4、MoO3、Fe2O3.Just
The mass ratio of negative electrode material is 5:1-1:5, preferred scope 2:1-1:2.
According to above scheme, the material of high conductivity is added in the positive and negative pole material that the present invention uses, such as graphene, charcoal
It is black, additional proportion 1wt%-20wt%, preferred scope 5wt%-15wt%.
According to above scheme, electrolyte that the present invention uses is liquid electrolyte, the quasi- solid-state electrolytic solution of gel and all solid state
Electrolyte.Wherein liquid electrolyte includes acid, neutral, alkalinity aqueous electrolyte；Cation mainly has glyoxaline cation, pyrrole
Pyridine cation, piperidines cation, pyrroles's cation, indoles cation, quaternary ammonium cation, trialkyl sulphur cation and other, yin
Ion mainly has iodide ion, bromide ion, chloride ion, tetrafluoroborate, hexafluorophosphate, nitrate anion, disulfate, trifluoromethyl
The example liquid electrolyte of sulfimide.The gelling agent of the quasi- solid-state electrolytic solution of gel includes PVA, PS and silica.It is all solid state
The gelling agent of electrolyte includes PEO etc..It is preferred that water system and PVA, PEO solid-state electrolytic solution.
According to above scheme, the preparation method of all solid state plane asymmetric miniature ultracapacitor device of the invention includes following
Step: firstly, mask plate is placed on filter paper, one layer of nonmetallic current collector material is filtered respectively at the both ends of mask plate；Its
It is secondary, anode film material is filtered in one end of mask plate, the other end filters negative film material；Later, mask plate is removed, by institute
The device of preparation is compacted or is transferred on tablet press machine in other flexible substrates；Finally, dripping upper electrolyte, encapsulation.
According to above-mentioned steps, the mask plate that the present invention uses is made on metal or plastic-substrates respectively using lithographic technique
Kind of hollow out figure is simultaneously accurately positioned, for use in a kind of structure of filtering, configuration include level-crossing finger-type, concentric ring type,
Parallel line type, parallel fold lines type, concentric interdigital.
According to above-mentioned steps, the pressure for the tablet press machine that the present invention uses is 5~50MPa, preferably 10~20MPa
According to above-mentioned steps case, encapsulating material of the invention includes flexible package and rigid package.The material of flexible package is PET；
Hard Roll package material is PMMA and organic glass, is specially cut into PMMA suitably sized, and it is asymmetric miniature to be placed on plane
Around supercapacitor, lid two panels organic glass piece is sealed against respectively up and down.
The present invention, which has the advantage that, proposes a kind of all solid state plane asymmetric miniature ultracapacitor device energy of raising
The thinking of density, i.e., by screening the usage amount of matched electrode material and material, so that two electrode materials are in charge and discharge
Different effects is given full play in journey, and two electrode materials are all not limited solely to the electric double layer adsorbed reaction, simultaneously
Fake capacitance reaction can occur, the successful match of selected electrode material realizes plane asymmetric miniature ultracapacitor device simultaneously
Purpose with height power density and energy density.In addition, asymmetric micro- using mask plate aided filter technology preparation plane
Type supercapacitor breaches traditional photo-etching processes, electrodeposition technology etc. time-consuming, technique is difficult to control, process is complicated
Limitation, processing cost greatly reduces, improves processing efficiency, quick, large batch of can prepare with specific several
The micro super capacitor of what configuration and size.The present invention can be widely used in MEMS, microrobot, miniature plant
Enter the micro-nano devices such as formula Medical Devices field.
Detailed description of the invention:
Fig. 1 mask plate aided filter method prepares plane asymmetric miniature ultracapacitor device flow chart.
Fig. 2 plane asymmetric miniature ultracapacitor device schematic diagram and electronic scanner microscope figure.
Fig. 3 present invention patterns anode and cathode configuration, and picture a-e is respectively level-crossing finger-type, concentric ring type, parallel
Line style, parallel fold lines type, concentric interdigital.
Fig. 4 plane asymmetric miniature ultracapacitor device performance map.
Specific embodiment:
Embodiment 1
Electrochemical stripping graphene (EG) ultrasonic disperse in ethanol solution, is configured to the dispersion of 0.1mg/mL first
Liquid；By Co (OH)2Mixed with EG (ratio be Co (OH)25wt%) ultrasound, be configured to the Co (OH) of 0.25mg/mL2/ EG dispersion
Liquid；VN and EG is mixed into (3wt% that ratio is VN) ultrasound, is configured to the VN/EG dispersion liquid of 0.25mg/mL.Then, by metal
Mask plate is placed on nylon filters, filters 0.5mL EG respectively as nonmetallic collector at the both ends of mask plate.In this base
Co (OH) is filtered in one end of mask plate on plinth2/ EG material, the other end filter VN/EG material, and the mass ratio of two kinds of materials is 1:
1.Mask plate is removed later, and prepared device is compacted on tablet press machine, pressure 5MPa.Finally, on the device of preparation
1M KOH electrolyte in drop, rigid package carry out electro-chemical test.
Embodiment 2
First by carbon nanotube ultrasonic disperse in ethanol solution, it is configured to the dispersion liquid of 0.1mg/mL；By hole graphene
Ultrasound arrangement at 0.25mg/mL dispersion liquid；By TiN ultrasound arrangement at the dispersion liquid of 0.25mg/mL.Then, by metal mask
Plate is placed on cellulose mixture filter membrane, filters 1mL carbon nanotube respectively as nonmetallic collector at the both ends of mask plate.?
In one end filter hole grapheme material of mask plate on the basis of this, the other end filters TiN material, and the mass ratio of two kinds of materials is 1:
1.5.Mask plate is removed later, and prepared device is compacted on tablet press machine, pressure 20MPa.Finally, in the device of preparation
PVA/KOH electrolyte in upper drop, rigid package carry out electro-chemical test.
Embodiment 3
First by PH1000 ultrasonic disperse in ethanol solution, it is configured to the dispersion liquid of 0.1mg/mL；By NiO and PH1000
Mixing ultrasound is configured to NiO/PH1000 (15wt% that ratio is NiO) dispersion liquid of 0.25mg/mL；By Mn3O4With PH1000
(ratio Mn3O410wt%) mixing ultrasound, be configured to the Mn of 0.25mg/mL3O4/ PH1000 dispersion liquid.Then, by metal
Mask plate is placed on nylon filters, filters 2mL PH1000 respectively as nonmetallic collector at the both ends of mask plate.Herein
On the basis of mask plate one end filter NiO/PH1000 material, the other end filter Mn3O4/ PH1000 material, the matter of two kinds of materials
Amount is than being 1:1.5.Mask plate is removed later, and prepared device is compacted on tablet press machine, pressure 5MPa.Finally, making
Upper PS-PEO/KOH electrolyte is dripped on standby device, rigid package carries out electro-chemical test.
Embodiment 4
First by EG ultrasonic disperse in ethanol solution, it is configured to the dispersion liquid of 0.1mg/mL；Active carbon is mixed with EG
Ultrasound is configured to active carbon/EG (10wt% that ratio is active carbon) dispersion liquid of 0.25mg/mL；By MnO2It is mixed with EG super
Sound is configured to the MnO of 0.25mg/mL2/ EG (ratio MnO215wt%) dispersion liquid.Then, metal mask plate is placed on
On cellulose mixture filter membrane, 0.5mL EG is filtered respectively as nonmetallic collector at the both ends of mask plate.Exist on this basis
One end filter activity charcoal/EG material of mask plate, the other end filter MnO2/ EG material, the mass ratio of two kinds of materials are 1:3.It
After remove mask plate, prepared device is transferred in PET base, pressure 15MPa.Finally, being dripped on the device of preparation
Upper 1M NaSO4Electrolyte, rigid package carry out electro-chemical test.
Embodiment 5
First by EG ultrasonic disperse in ethanol solution, it is configured to the dispersion liquid of 0.1mg/mL；By MnO2It is mixed with EG super
Sound is configured to the MnO of 0.25mg/mL2/ EG dispersion liquid；By MoO3Ultrasound is mixed with EG, is configured to the MoO of 0.25mg/mL3/EG
Dispersion liquid.Then, metal mask plate is placed on nylon filters, filters 0.5mL EG respectively as non-at the both ends of mask plate
Metal collector.MnO is filtered in one end of mask plate on this basis2/ EG material, the other end filter MoO3/ EG material, two kinds
The mass ratio of material is 1:2.5.Mask plate is removed later, and prepared device is transferred on polyethylene diagrams under stress,
Pressure is 15MPa.Finally, dripping upper PVA/NaSO on the device of preparation4Electrolyte, flexible package carry out electro-chemical test.
Claims (10)
1. a kind of all solid state plane asymmetric miniature ultracapacitor device, it is characterised in that:
(1) micro super capacitor mainly includes following sections: flexible substrates, and the patterning being deposited in substrate is nonmetallic
Collector positioned at the positive electrode and negative electrode material of nonmetallic collection liquid surface, and is covered in anode and cathode region
On electrolyte；
(2) after the patterned positive electrode of flexible substrates and the coating of negative electrode material region part or electrolyte being added dropwise,
It is encapsulated, that is, prepare all solid state plane asymmetric miniature ultracapacitor device.
2. all solid state plane asymmetric miniature ultracapacitor device according to claim 1, it is characterised in that: the flexibility
Substrate include various filter paper (cellulose mixture film or nylon membrane etc.), polyethylene terephthalate (PET) film, polyethylene every
Film, polypropylene diaphragm, paper or textile material；
The nonmetallic collector be good conductivity, smooth material, such as graphene, carbon nanotube, polyethylene diformazan thiophene:
One of polystyrolsulfon acid (PH1000) or two kinds or more, with a thickness of 10nm-10 μm.
3. all solid state plane asymmetric miniature ultracapacitor device according to claim 1, it is characterised in that: the pattern
The configuration of polarizing electrode includes level-crossing finger-type, concentric ring type, parallel line type, parallel fold lines type, concentric interdigital, miniature super
The size of grade capacitor is 10 μm of -10cm, with a thickness of 100nm-200 μm.
4. all solid state plane asymmetric miniature ultracapacitor device according to claim 1 or 3, it is characterised in that: described
Positive electrode includes graphene, active carbon, carbon nanotube, Co (OH)2、Ni(OH)2、Co3O4、MnO2One of or two kinds with
On, negative electrode material includes graphene, active carbon, carbon nanotube, VN, TiN, Mn3O4、MoO3、Fe2O3；Positive electrode and cathode material
The mass ratio of material is 5:1-1:5.
5. all solid state plane asymmetric miniature ultracapacitor device according to claim 1 or 4, it is characterised in that positive electrode
With the material for being separately added into high conductivity in negative electrode material, such as one of graphene, conductive black or two kinds, additional proportion is
The 0wt%-20wt% of positive or negative pole material.
6. all solid state plane asymmetric miniature ultracapacitor device according to claim 1, it is characterised in that the electrolysis
Liquid is one of liquid electrolyte, the quasi- solid-state electrolytic solution of gel or all solid state electrolyte；Wherein liquid electrolyte include it is acid,
Neutral, alkalinity aqueous electrolyte；Cation mainly have glyoxaline cation, pyridylium, piperidines cation, pyrroles's sun from
Son, indoles cation, quaternary ammonium cation, trialkyl sulphur cation and other one of or two kinds or more, anion mainly has
Iodide ion, bromide ion, chloride ion, tetrafluoroborate, hexafluorophosphate, nitrate anion, disulfate, in trifluoromethanesulp-onyl -onyl imide
One or two or more kinds of il electrolytes；The gelling agent of the quasi- solid-state electrolytic solution of gel includes polyvinyl alcohol (PVA), gathers
One of styrol copolymer (PS) and silica or two kinds or more；The gelling agent of all solid state electrolyte includes polyoxyethylene
Alkene (PEO).
7. a kind of preparation method of any all solid state plane asymmetric miniature ultracapacitor device of claim 1-6, special
Sign is the following steps are included: using mask plate aided filter method, firstly, mask plate is placed on flexible filter paper, in mask
One layer of nonmetallic current collector material is filtered respectively in the both ends of plate；Secondly, anode film material is filtered in one end of mask plate, it is another
End filtering negative film material；Later, mask plate is removed, prepared device is compacted on tablet press machine or turns to be pressed onto other is soft
In property substrate；Finally, being powered in the patterned positive electrode of flexible substrates and the coating of negative electrode material region part or drop
Xie Zhi, encapsulation.
8. the preparation method of all solid state plane asymmetric miniature ultracapacitor device according to claim 7, mask plate is benefit
Various hollow out figure are made on metal or plastic-substrates of lithographic technique and are accurately positioned, for use in a kind of knot of filtering
Structure, configuration include one of level-crossing finger-type, concentric ring type, parallel line type, parallel fold lines type, concentric interdigital.
9. the preparation method of all solid state plane asymmetric miniature ultracapacitor device according to claim 7, the pressure of tablet press machine
Power is 5~50MPa.
10. the preparation method of all solid state plane asymmetric miniature ultracapacitor device according to claim 7, encapsulation includes soft
Packaging or rigid package, flexible package encapsulating material are PET package；Hard Roll package material is polymethyl methacrylate (PMMA) and organic
PMMA, is specially cut into suitably sized by glass, is placed on around plane asymmetric miniature ultracapacitor device, up and down point
Not lid two panels organic glass piece is sealed against.
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| CN110970232A (en) * | 2019-11-25 | 2020-04-07 | 中山大学 | Stretchable microelectronic device with hydrogel as substrate and preparation method thereof |
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| CN110911171B (en) * | 2019-11-26 | 2021-11-09 | 东华大学 | Asymmetric microchip supercapacitor and preparation method thereof |
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Application publication date: 20190115 |