CN108682651A - A kind of flexible electrode and preparation method thereof based on dendritic nano-silver structure - Google Patents
A kind of flexible electrode and preparation method thereof based on dendritic nano-silver structure Download PDFInfo
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- CN108682651A CN108682651A CN201810500824.3A CN201810500824A CN108682651A CN 108682651 A CN108682651 A CN 108682651A CN 201810500824 A CN201810500824 A CN 201810500824A CN 108682651 A CN108682651 A CN 108682651A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
- H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
- H01L21/76838—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the conductors
- H01L21/76886—Modifying permanently or temporarily the pattern or the conductivity of conductive members, e.g. formation of alloys, reduction of contact resistances
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/46—Electroplating: Baths therefor from solutions of silver
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/02—Electroplating of selected surface areas
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/18—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material
- H05K3/188—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material by direct electroplating
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- Power Engineering (AREA)
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- Non-Insulated Conductors (AREA)
- Manufacturing Of Electric Cables (AREA)
- Parts Printed On Printed Circuit Boards (AREA)
Abstract
The present invention relates to a kind of flexible electrode and preparation method thereof based on dendritic nano-silver structure, belongs to flexible electronics technical field.Main technical schemes are as follows：First produce the stickup with circuit pattern structure, then it will be attached on the indium oxide tin glass by stratiform alternating deposit, one layer of nano-silver conductive layer that there is circuit pattern and have dendroid appearance structure is deposited by the method for electrochemical deposition, and this layer of nano-silver conductive layer is solidificated on PDMS, prepare the flexible circuit with dendritic structure nano silver.Preparation method is simple, reproducible by the present invention, need not be synthetically prepared, and overcomes and is synthesized in traditional handicraft and detach the technical difficulty in nano silver, while can solve the problems, such as to encounter in nano silver coating.The circuit of preparation has lower sheet resistance, and remains to keep good electric conductivity after bending is multiple and tape-stripping is multiple.
Description
Technical field
The present invention relates to flexible electronics technical fields, and in particular to a kind of based on embedding dendritic nano-silver structure
The preparation method of flexible circuit
Background technology
Present electronic equipment and electronic device is all based on rigid and crisp material, with smart home and wearable
The development of Medical Devices, people gradually produce keen interest to electronic equipment flexible.Next-generation electronic equipment is becoming
Develop in the direction of lighting, flexibility, meandering.There are many research of flexible electrode material at present, but in the prevalence of not
It is wear-resisting, the problems such as bendability is poor, and electric conductivity is bad.Therefore, there is superpower resistance to bend(ing), wearability, the material of satisfactory electrical conductivity
Material is the hot spot of this field developmental research.
About the exploitation of flexible transparent conductive film, flexible wear circuit, this field is just started to walk.Although in recent years,
People attempt to prepare flexible circuit with nano-particle, carbon nanotube and graphene, but they that there is circuit-making process is multiple
It is miscellaneous, circuit conductive is bad and circuit not durable wear the problems such as.Therefore, high-performance flexible transparent conductive film, flexible wear
Circuit research and development are most important to the development of flexible electronic devices.
Invention content
In order to solve the above technical problems, the purpose of the present invention is to provide one kind having both superior electrical conductivity, excellent abrasive resistance
With the flexible circuit and preparation method thereof based on embedding dendritic nano-silver structure of resistance to bend(ing).
The present invention inventive concept be：The stickup with circuit pattern structure is first produced, then stickup is attached to and is being passed through
It crosses on tin indium oxide (ITO) glass of stratiform alternating deposit, depositing one layer by the method for electrochemical deposition has circuit diagram
Case and the nano-silver conductive layer for having dendroid appearance structure, and this layer of nano-silver conductive layer is solidificated on PDMS, preparation is provided
There is the novel flexible circuit of dendritic structure nano silver.Such flexible circuit has a clearly circuit structure, lower sheet resistance, and
And it remains to keep good electric conductivity after multiple bending and tape-stripping.
To achieve the above object, flexible circuit preparation method of the present invention is as follows：
(1) stickup with circuit pattern is marked out, the pattern and width of circuit can design as needed；
(2) by ito glass LBL self-assembly, stickup is sticked on assembled ito glass, then removes circuit pattern
It pastes and exposes ito glass, ito glass is put into electrolyte and carries out electrochemical deposition, after electrochemical deposition, white branch
Shape nano silver will be deposited on the circuit of ito glass, be called ITO-Ag-circuits；
(2) ITO-Ag-circuits is immersed in the PDMS with curing agent (dimethyl silicone polymer) solution, heating is solid
Change, the PDMS flexible substrates being cured are taken off from ITO-Ag-circuits, the white dendroid nanometer with circuit pattern
Silver is embedded in PDMS to get dendritic nano-silver flexible circuit PDMS-Ag-circuits.
Preferably, electrolyte is AgNO in the step (1)3And NaNO3Mixed solution, AgNO3A concentration of 0.005~
0.015mol/L, NaNO3A concentration of 0.01~0.12mol/L, reference electrode are saturation Mercurous sulfate electrode, are platinum to electrode
Silk, working electrode are assembled ito glass.
Preferably, the self assembly number of plies is 4~10 layers in the step (1).
Preferably, the electrochemical deposition time is 1000~5000s, the current potential of electrochemical deposition setting in the step (1)
Ranging from (- 0.6)~(- 0.3) V.
Preferably, PDMS stostes and the volume ratio of curing agent are 10 in the step (2)：1.
Preferably, the solidification temperature is 50~100 DEG C, and hardening time is 2~10 hours.
The ito glass further includes cleaning treatment before patch stickup and self assembly, and cleaning process is to use ito glass respectively
Deionized water, acetone and EtOH Sonicate clean 20~40 minutes.It is put into after cleaning in ozone clean machine and carries out surface hydroxylation.Through
It crosses after above-mentioned cleaning treatment again by ito glass in PDDA (diallyl dimethyl ammoniumchloride) and PSS (polystyrolsulfon acids
Sodium) LBL self-assembly is carried out in solution.
Compared with prior art, the invention has the advantages that：(1) circuit-making process of the present invention is simple, Yi Shi
Existing volume production.(2) circuit of the present invention is easily designed, and electric conductivity is excellent, wear-resisting property is strong, bendability is good, Portable durable.(3)
Preparation method of the present invention can Direct precipitation go out the shape of circuit, do not need the circuit production in later stage, it is simple and practicable.(4) of the invention
Dendritic nano-silver, structure has numerous branch fork structures so that contact area increases between nano silver branch, is conducive to increase
Electron-transport, and then electrode resistance is reduced, good electric conductivity is the guarantee for preparing good dice.(5) present invention uses
Prepare the electrochemical deposition method of dendritic nano silver, sharpest edges are simple and practicable, reproducible, need not synthesize system
It is standby, it overcomes and is synthesized in traditional handicraft and detach the technical difficulty in nano silver, while can solve to encounter in nano silver coating
Problem.
Description of the drawings
Fig. 1 is present invention process flow chart；
Fig. 2 is the sem image of flex circuit surface nano-silver conductive layer made according to the method for the present invention；
Fig. 3 is linear type circuit bright light pictorial diagram of the embodiment of the present invention；
Fig. 4 is the arcuate electrode of the embodiment of the present invention；
Fig. 5 is dendritic nano-silver circuit.
Specific implementation mode
The present invention is described in detail below by specific embodiment, but is not limited the scope of the invention.Unless otherwise specified, originally
Experimental method is conventional method used by invention, and experiment equipment used, material, reagent etc. commercially obtain.
Embodiment 1
Circuit pattern is designed, marking one is straight with two 2mm (width) x 6cm (length) in the stickup that can remove pattern
Item.
Ito glass is cleaned before assembly, and cleaning process is that ito glass is used deionized water, acetone respectively
It is cleaned 30 minutes with EtOH Sonicate.It is put into after cleaning in ozone clean machine and carries out surface hydroxylation.Then ito glass is existed again
LBL self-assembly is carried out in PDDA (diallyl dimethyl ammoniumchloride), PSS (kayexalate) solution, by ITO glass
Glass carries out 6 layers of self assembly, a concentration of 0.1~10mg/mL of wherein PDDA, preferably 1mg/mL；PSS solution concentrations be 0.1~
10mg/mL, preferably 1mg/mL.
Stickup is attached on assembled ito glass, then the part of two vertical bars of removal circuit, on ito glass only
Two straight bars sections are exposed ITO, and ito glass is put into AgNO3And NaNO3In mixed solution, using ito glass as work
Electrode, the method used is chronoamperometry, to be saturated Mercurous sulfate electrode as reference electrode, with platinum filament to electrode, when deposition
Between be 1000s, AgNO3A concentration of 0.008mol/L, NaNO3A concentration of 0.1mol/L sets current potential as -0.3V.Pass through electrochemistry
Deposition, prepares two white nano-silver conductive layers on ito glass surface, is observed that by microscope or scanning electron microscope
Its dendroid microscopic appearance structure.
The other parts for gently removing stickup are put into baking oven by the ito glass merging PDMS solution after deposition nano silver
Middle solidification, solidification temperature are 70 DEG C, and hardening time is 5 hours.The PDMS being cured is taken off from ito glass, dendroid is received
The silver-colored circuit of rice is fixed in PDMS, and the dendritic structure (as shown in Figure 2) of PDMS nano surface silver can be observed by Electronic Speculum.
The PDMS circuits of the dendritic structure nano silver with two direct-wire circuits obtained can be used as superpower resistance to bend(ing), wear-resisting
Property, the telegraph circuit of satisfactory electrical conductivity.
Electric conductivity test is carried out to the telegraph circuit of preparation, circuit on one side is connected to the two poles of the earth of LED bulb, other end connects
The two poles of the earth of battery are connect, as shown in figure 3, transparent circuitry has superpower tough bendability and LED bulb normal luminous, illustrate dendritic silver
The electric conductivity of vertical bar type circuit is good.
Embodiment 2
Circuit pattern is designed, one arch with a 2mm (width) of marking can remove the stickup of pattern.
Ito glass is cleaned 30 minutes with deionized water, acetone and EtOH Sonicate respectively.Ozone clean machine is put into after cleaning
In carry out surface hydroxylation.Then ito glass in PDDA and PSS solution is subjected to LBL self-assembly again, ito glass is carried out
6 layers of self assembly.
Stickup is attached on assembled ito glass, the bowed part of circuit is then removed, only bends on ito glass
Shape part is exposed ITO, and ito glass is put into AgNO3And NaNO3In mixed solution, using ito glass as working electrode, use
Method be chronoamperometry, to be saturated Mercurous sulfate electrode as reference electrode, with platinum filament to electrode, sedimentation time 2000s,
AgNO3A concentration of 0.008mol/L, NaNO3A concentration of 0.1mol/L sets current potential as -0.3V.By electrochemical deposition, in ITO
Glass surface prepares the nano silver circuit of bow-shaped structural.
The other parts for gently removing stickup are put into baking oven by the ito glass merging PDMS solution after deposition nano silver
Middle solidification, solidification temperature are 70 DEG C, and hardening time is 5 hours.The PDMS being cured is taken off from ito glass, dendroid is received
The silver-colored circuit of rice is fixed in PDMS, and the PDMS circuits of the dendritic structure nano silver of the arch circuit (such as Fig. 4) obtained are i.e.
It can be used as superpower resistance to bend(ing), wearability, the arcuate electrode circuit of satisfactory electrical conductivity.
Embodiment 3
Circuit pattern is designed, marking one has a plurality of 2mm wide, the set pattern of different length broken line pattern circuit viscous
Patch.
Ito glass is cleaned 30 minutes with deionized water, acetone and EtOH Sonicate respectively.Ozone clean machine is put into after cleaning
In carry out surface hydroxylation.Then ito glass in PDDA and PSS solution is subjected to LBL self-assembly again, ito glass is carried out
6 layers of self assembly.
Stickup is attached on assembled ito glass, circuit part is then removed, only broken line circuit is on ito glass
Ito glass is put into AgNO by exposed ITO3And NaNO3In mixed solution, using ito glass as working electrode, the method that uses for
Chronoamperometry, to be saturated Mercurous sulfate electrode as reference electrode, with platinum filament to electrode, sedimentation time 3000s, AgNO3It is dense
Degree is 0.008mol/L, NaNO3A concentration of 0.1mol/L sets current potential as -0.3V.By electrochemical deposition, in ito glass table
Prepare the nano silver circuit with various meander line structures in face.
The other parts for gently removing stickup are put into baking oven by the ito glass merging PDMS solution after deposition nano silver
Middle solidification, solidification temperature are 70 DEG C, and hardening time is 5 hours.The PDMS being cured is taken off from ito glass, dendroid is received
The silver-colored circuit of rice is fixed in PDMS, and the PDMS circuits of the dendritic structure nano silver of a plurality of broken line circuit obtained can be made
For superpower resistance to bend(ing), wearability, the broken line circuit set of satisfactory electrical conductivity.
Embodiment 4
Marking one has a plurality of 2mm wide, the set pattern stickup of different bending angles and radius pattern circuit.
Ito glass is cleaned 40 minutes with deionized water, acetone and EtOH Sonicate respectively.Ozone clean machine is put into after cleaning
In carry out surface hydroxylation.Then ito glass in PDDA and PSS solution is subjected to LBL self-assembly again, ito glass is carried out
10 layers of self assembly.
Stickup is attached on assembled ito glass, circuit part is then removed, only broken line circuit is on ito glass
Ito glass is put into AgNO by exposed ITO3And NaNO3In mixed solution, using ito glass as working electrode, the method that uses for
Chronoamperometry, to be saturated Mercurous sulfate electrode as reference electrode, with platinum filament to electrode, sedimentation time 4800s, AgNO3It is dense
Degree is 0.005mol/L, NaNO3A concentration of 0.0.005mol/L sets current potential as -0.6V.By electrochemical deposition, in ITO glass
Prepare the nano silver circuit with various sweep structures in glass surface.
The other parts for gently removing stickup are put into baking oven by the ito glass merging PDMS solution after deposition nano silver
Middle solidification, solidification temperature are 100 DEG C, and hardening time is 10 hours.The PDMS being cured is taken off from ito glass, dendroid
Nano silver circuit is fixed in PDMS, the PDMS circuits of the dendritic structure nano silver of a plurality of curve circuit obtained
As superpower resistance to bend(ing), wearability, the curve circuit set of satisfactory electrical conductivity.
Resistive performance test is carried out to the sample that embodiment 1-4 is obtained, we test the original resistance of circuit, bending 90
The resistance that degree is 1000 times, with 500 resistance of 3M tape-strippings, parameter difference is as shown in table 1.
Table 1：The electric conductivity of flexible circuit
| Sample | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Original sheet resistance (ohm/sq) | 3.10 | 0.99 | 0.48 | 1.80 |
| Bend 90 degree of 1000 sheet resistances (ohm/sq) | 5.45 | 1.65 | 0.76 | 2.98 |
| With 500 sheet resistances (ohm/sq) of 3M tape-strippings | 4.21 | 1.24 | 0.55 | 2.10 |
The data from table 1 are it is found that the flexible circuit gradually increases with the increase resistance of bending number, with 3M tape-strippings
After 500 times, sheet resistance just slightly rises, and on the whole the circuit has lower sheet resistance, and is being bent multiple and tape-stripping
It remains to keep good electric conductivity after repeatedly.
The preferable specific implementation mode of the above, only the invention, but the protection domain of the invention is not
It is confined to this, any one skilled in the art is in the technical scope that the invention discloses, according to the present invention
The technical solution of creation and its inventive concept are subject to equivalent substitution or change, should all cover the invention protection domain it
It is interior.
Claims (8)
1. a kind of flexible electrode based on dendritic nano-silver structure, which is characterized in that including PDMS flexible and be embedded in
Dendritic nano-silver in PDMS.
2. a kind of preparation method of flexible electrode as described in claim 1, which is characterized in that include the following steps：
(1) stickup with circuit pattern is marked out, the pattern and width of circuit can design as needed；
(2) by ito glass LBL self-assembly, stickup is sticked on assembled ito glass, then removes the stickup of circuit pattern
Expose ito glass, ito glass is put into electrolyte and carries out electrochemical deposition, after electrochemical deposition, white dendroid is received
Meter Yin will be deposited on the circuit of ito glass, be called ITO-Ag-circuits；
(2) ITO-Ag-circuits is immersed in the PDMS solution with curing agent, is heating and curing, the PDMS being cured is soft
Property substrate taken off from ITO-Ag, the white dendritic nano-silver with circuit pattern is embedded in PDMS and is received to get dendroid
The silver-colored flexible circuit PDMS-Ag-circuits of rice.
3. according to the method described in claim 2, it is characterized in that, electrolyte is AgNO in the step (1)3And NaNO3Mixing
Solution, AgNO3A concentration of 0.005~0.015mol/L, NaNO3A concentration of 0.01~0.12mol/L, reference electrode are saturation sulphur
Sour mercurous electrode, is platinum filament to electrode, and working electrode is assembled ito glass.
4. according to the method described in claim 2, it is characterized in that, the self assembly number of plies is 4~10 layers in the step (1).
5. according to the method described in claim 2, it is characterized in that, in the step (1) the electrochemical deposition time be 1000~
5000s, the potential range that electrochemical deposition is set is (- 0.6)~(- 0.3) V.
6. according to the method described in claim 2, it is characterized in that, in the step (2) PDMS stostes and curing agent volume
Than being 10：1.
7. according to the method described in claim 2, it is characterized in that, the solidification temperature be 50~100 DEG C, hardening time 2
~10 hours.
8. according to the method described in claim 2, it is characterized in that, the ito glass cleaning process is to use ito glass respectively
Deionized water, acetone and EtOH Sonicate clean 20~40 minutes, are put into after cleaning in ozone clean machine and carry out surface hydroxylation.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109493998A (en) * | 2018-12-17 | 2019-03-19 | 太原理工大学 | A kind of flexible transparent conducting film and preparation method thereof based on patterning layer assembly self-supporting film |
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| CN102181891A (en) * | 2011-04-08 | 2011-09-14 | 温州大学 | Silver nanodendrite surface enhanced Raman scattering (SERS) substrate, and preparation method and application thereof |
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Application publication date: 20181019 |