CN109298045A - A kind of silver nanowires based on PDMS/nanogold combination electrode and preparation method thereof - Google Patents
A kind of silver nanowires based on PDMS/nanogold combination electrode and preparation method thereof Download PDFInfo
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- CN109298045A CN109298045A CN201811240192.8A CN201811240192A CN109298045A CN 109298045 A CN109298045 A CN 109298045A CN 201811240192 A CN201811240192 A CN 201811240192A CN 109298045 A CN109298045 A CN 109298045A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
Abstract
The present invention relates to the silver nanowires based on PDMS/nanogold combination electrodes and preparation method thereof.Silver nanowires based on the PDMS/nanogold combination electrode includes: that PDMS is substrate, and silver nanowires is conductive layer, and nanogold particle is electrochemical deposition layer, and the nanogold particle is deposited in silver nanowires.Silver nanowires of the present invention/nanogold combination electrode, has the characteristics that low resistance, high-mechanical property, resistance range: 0.5 Ω sq‑1~11 Ω sq‑1, the resistance range after bending 500 times: 0.9 Ω sq‑1~16 Ω sq‑1, resistance range after stretching 100 times: 0.8 Ω sq‑1~10 Ω sq‑1, performance is at the leading level in the same industry, electronic component miniaturization and it is integrated in have a good application prospect.
Description
Technical field
The present invention relates to electrochemical sensor fields, and in particular to a kind of flexible silver nanowires/nanogold based on PDMS
Combination electrode and preparation method thereof.
Background technique
Nowadays, flexible transparent electrode occupies very important status in the development of electronics and photoelectronic industry, is system
Standby numerous electronics and the indispensable photoelectric functional material of photoelectron element.But the indium tin oxide transparent being commonly used is led
Electric material raw material phosphide element reserves are limited, expensive, and itself is not bent, and nano-silver thread has good resist bending
Property, electric conductivity and thermal conductivity, be the good selection for making flexible and transparent conductive material.
Nanogold has unique physicochemical properties, excellent optics, chemistry, physics, electrical properties and biology parent
And property becomes biological neck so that it has been to be concerned by more and more people and pay attention in terms of the analysis detection of biochemical field
Domain, chemical field, physical field a research hotspot.
Electrochemical deposition is the method when former commonly controls preparation nano material, and reaction condition is easier, can
By controlling electrochemical deposition current potential, deposition current, sedimentation time, the concentration of electrolyte of deposition and surfactant agent etc. no
The structures such as nano metal, Nano semiconductor and the nanometer conductive polymer of a large amount of different size patterns can be synthesized with conditions.
Summary of the invention
Simple, the low-cost flexibility silver based on PDMS is made technical problem to be solved by the invention is to provide a kind of
Nano wire/nanogold combination electrode, can be used as the working electrode of use for electrochemical tests.
In order to solve the above technical problems, the present invention provides a kind of silver nanowires based on PDMS/nanogold combination electrode.It should
Electrode includes: using PDMS as substrate, and silver nanowires is conductive layer, and nanogold particle is electrochemical deposition layer, the nanogold
Grain is deposited in silver nanowires.
And the method for preparing a kind of above-mentioned silver nanowires based on PDMS/nanogold combination electrode, this method comprises:
S1: in the PDMS monomer that the silicon wafer template upper mass ratio obtained by photolithography method is 1:1-20:1 and cause liquid
Mixed solution obtains the PDMS substrate of fixed shaped recesses after heated solidification；
S2: the PVP mixed solution that the PVA and mass concentration that configuration quality concentration is 0.1%-10% are 0.1%-10%,
The PDMS substrate that S1 is prepared is soaked in PVA and PVP mixed solution, after heated solidification, obtains the PDMS of surface hydrophilic
Substrate；
S3: by silver nanowires ethanol solution that concentration is 0.01-10mg/mL (silver nanowires and ethyl alcohol volume ratio 10:1~
1:1), in the groove for equably spreading over the surface PDMS, PDMS-AgNWs conductive layer, the silver nanowires length 50- are obtained
200nm, diameter 30-100nm；
S4: 0.1~5mg/mL KAuCl is immersed using PDMS-AgNWs as working electrode4With 0.1~1mol/L H2SO4's
In mixed electrolytic solution, reference electrode is Ag/AgCl electrode, and auxiliary electrode is platinum filament, and it is heavy to carry out constant potential using chronoamperometry
Product, deposition current are -0.3~-3mA, 10~1600s of sedimentation time.Obtain PDMS-AgNWs-AuNPs silver nanowires/nanogold
Combination electrode.
Preferably, in step sl, the matter of the monomer of the PDMS mixed liquor being cast in silicon wafer template and initiation liquid
Amount is than being 10:1.
Preferably, in step sl, it needs to pump the gas in PDMS mixed solution by negative pressure before heat-curing step
The step of bubble, needs the step of cleaning by UV ozone after heat-curing step.
Preferably, in step s 2, in the mixed liquor of the PVA and PVP, the concentration that PVA concentration is 4%, PVP is 7%.
Preferably, in step s3, the concentration of the silver nanowires solution is 5mg/mL.
Flexibility silver nanowires/nanogold combination electrode prepared by the present invention, has the characteristics that low resistance, high-mechanical property,
Resistance range: 0.5 Ω sq-1~11 Ω sq-1, the resistance range after bending 500 times: 0.9 Ω sq-1~16 Ω sq-1, stretch 100 times
Resistance range afterwards: 0.8 Ω sq-1~10 Ω sq-1。
Flexible silver nanowires/nanogold combination electrode performance prepared by the method for the present invention is in a leading position in the same industry
Level, electronic component miniaturization and it is integrated in have a good application prospect.
Detailed description of the invention
Attached drawing 1 is the silver nanowires based on PDMS/nanogold combination electrode planar structure schematic diagram.
Attached drawing 2 is silver nanowires/nanogold combination electrode surface topography map.
Attached drawing 3 is chemical property figure after silver nanowires/nanogold combination electrode bending.
Attached drawing 4 is chemical property figure after silver nanowires/nanogold combination electrode stretches.
Attached drawing 5 is resistance measurement figure after silver nanowires/nanogold combination electrode stretches.
Attached drawing 6 is resistance measurement figure after silver nanowires/nanogold combination electrode bending.
Specific embodiment
Below in conjunction with attached drawing, the present invention is further illustrated.
Silver nanowires based on PDMS/nanogold combination electrode planar structure schematic diagram as shown in Figure 1.The electrode packet
Include: using PDMS as substrate, silver nanowires is conductive layer, and nanogold particle is electrochemical deposition layer, the nanogold particle deposition
In silver nanowires.
Novel silver nanowires/nanogold combination electrode performance quality depends on silver nanowires and is distributed on flexible substrates surface
With the uniformity coefficient of overlapped uniformity coefficient and gold nano grain size and distribution.As shown in Fig. 2, silver nanowires is in flexible electrode
Surface is evenly distributed, and overlap joint is close；It gold nano grain size and is evenly distributed.Illustrate that the novel electrode is functional.
Below with the preparation method for the specific silver nanowires based on the PDMS/nanogold combination electrode enumerated to the present invention
It is described further.
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention.In following embodiments unless otherwise specified, used experimental method is conventional method, used
Material, reagent etc. can chemically company be bought.
Embodiment 1
(1) PDMS (dimethyl silicone polymer) substrate makes.Substrate is made using photoetching technique.Electronic palette is used first
Software design electrode drawing, and drawing is printed into mask plate using photoetching mask-making technology, secondly revolved in clean silicon chip surface
Resist coating covers the mask plate containing electrode pattern, is finally exposed and develops, obtain silicon wafer template.Place it in one
In secondary property culture dish；Casting quality is than the PDMS mixed solution for 10:1 on it；Negative pressure in vacuum desiccator is placed into pump
Bubble in PDMS mixed solution, used time 2h；The 1h of being heating and curing is put into 80 DEG C of constant temperature oven after taking-up；By ready-made substrate
The dust that surface attachment is removed with 3M adhesive tape (being purchased from Minnesota Mining and Manufacturing Company) processing, is then placed in UV ozone cleaning machine and cleans
10min obtains the PDMS substrate with fixed shaped recesses.
(2) PDMS hydrophilic layer is modified.Specific step is as follows: 1. prepare mass percent be 4%PVA (polyvinyl alcohol) with
The water mixed solution of 7%PVP (polyvinylpyrrolidone)；2. the PDMS substrate prepared is soaked in PVA and PVP mixed solution
Middle 20min places into dry 1.5h in 80 DEG C of vacuum drying oven；3. it is 2. primary to repeat step；4. being then placed in 100 DEG C of vacuum
Heat fixation 20min in baking oven.5. it is 2. and 4. primary to repeat step, the PDMS substrate of surface hydrophilic is obtained.
(3) prepared by PDMS-AgNWs conductive layer.Compound concentration is the silver nanowires ethanol solution of 5mg/mL, silver nanoparticle line gauge
Lattice are as follows: diameter 90nm, 60 μM of length.In the groove for equably spreading over the surface PDMS, place at room temperature drying for one day.
(4) PDMS-AgNWs-AuNPs silver nanowires/nanogold combination electrode preparation.Using PDMS-AgNWs as work
Electrode immerses 5mg/ml KAuCl4With 0.5mol/L H2SO4Mixed electrolytic solution in, reference electrode be Ag/AgCl electrode, auxiliary
Electrode is platinum filament, carries out potentiostatic electrodeposition using chronoamperometry, carries out permanent electricity using the chronoamperometry of electrochemical workstation
Stream deposition, deposition voltage are -0.2V, sedimentation time 1600s.It places at room temperature drying for one day, that is, prepares silver nanowires/nanometer
Golden combination electrode.
(5) silver nanowires obtained/nanogold combination electrode is bent 500 times, each bending angle is 180 °.It is bending
In 5mM K after 100 times, 200 times, 300 times, 400 times, 500 times3[Fe(CN)6] in carry out cyclic voltammetric characterization, sweep speed
For 0.1mV/s, the current value of oxidation peak is recorded, as shown in Fig. 3, novel electrode is during bending 100 times to 500 times, electricity
The flexibility of pole keeps good, and electrochemistry is able to maintain stabilization after bending.
Embodiment 2
(1) PDMS substrate makes.Substrate is made using photoetching technique.Electronic palette software design electrode figure is used first
Paper, and drawing is printed into mask plate using photoetching mask-making technology, secondly in clean silicon chip surface spin coating photoresist, masking contains
There is the mask plate of electrode pattern, be finally exposed and develop, obtains silicon wafer template.It places it in batch cultur ware；?
Casting quality is than the PDMS mixed solution for 10:1 thereon；Negative pressure in vacuum desiccator is placed into pump in PDMS mixed solution
Bubble, used time 2h；The 1h of being heating and curing is put into 80 DEG C of constant temperature oven after taking-up；Ready-made substrate is handled with 3M adhesive tape and is removed
The dust of surface attachment, is then placed in UV ozone cleaning machine and cleans 10min, obtains the PDMS base with fixed shaped recesses
Piece.
(2) PDMS hydrophilic layer is modified.Reference literature simultaneously does some improvement, the specific steps are as follows: 1. prepares mass percent
For the water mixed solution of 4%PVA and 7%PVP；2. the PDMS substrate prepared is soaked in PVA and PVP mixed solution
20min places into dry 1.5h in 80 DEG C of vacuum drying oven；3. it is 2. primary to repeat step；4. being then placed in 100 DEG C of vacuum to dry
Heat fixation 20min in case.5. it is 2. and 4. primary to repeat step, the PDMS substrate of surface hydrophilic is obtained.
(3) prepared by PDMS-AgNWs conductive layer.Compound concentration is the silver nanowires ethanol solution of 5mg/mL, silver nanoparticle line gauge
Lattice are as follows: diameter 90nm, 60 μM of length.In the groove for equably spreading over the surface PDMS, place at room temperature drying for one day.
(4) PDMS-AgNWs-AuNPs silver nanowires/nanogold combination electrode preparation.Using PDMS-AgNWs as work
Electrode immerses 5mg/ml KAuCl4With 0.5mol/L H2SO4Mixed electrolytic solution in, reference electrode be Ag/AgCl electrode, auxiliary
Electrode is platinum filament, carries out potentiostatic electrodeposition using chronoamperometry, carries out permanent electricity using the chronoptentiometry of electrochemical workstation
Stream deposition, deposition current are -0.2V, sedimentation time 1600s.It places at room temperature drying for one day, that is, prepares silver nanowires/nanometer
Golden combination electrode.
(5) silver nanowires obtained/nanogold combination electrode is stretched 100 times, each tensile elongation is original length
30%.In 5mM K after stretching 20 times, 40 times, 60 times, 80 times, 100 times3[Fe(CN)6] in carry out cyclic voltammetric characterization, sweep
Retouching rate is 0.1mV/s, records the current value of oxidation peak, as shown in Fig. 4, novel electrode is in 20 times to 100 times mistakes of curved stretching
Cheng Zhong, the flexibility of electrode keep good, and electrochemistry is able to maintain stabilization after stretching.
Embodiment 3
(1) PDMS (dimethyl silicone polymer) substrate makes.Electronic palette software design electrode drawing, and benefit are used first
Drawing is printed into mask plate with optical graving version technique, secondly in clean silicon chip surface spin coating photoresist, masking contains electrode
The mask plate of figure, is finally exposed and develops, and obtains silicon wafer template.It places it in batch cultur ware；It pours on it
Infuse the PDMS mixed solution that mass ratio is 10:1；It places into negative pressure in vacuum desiccator and pumps bubble in PDMS mixed solution,
Used time 2h；The 1h of being heating and curing is put into 80 DEG C of constant temperature oven after taking-up；Ready-made substrate is handled with 3M adhesive tape and removes surface
The dust of attachment is then placed in UV ozone cleaning machine and cleans 10min, obtains the PDMS substrate with fixed shaped recesses.
(2) PDMS hydrophilic layer is modified.Reference literature simultaneously does some improvement, the specific steps are as follows: 1. prepares mass percent
For the water mixed solution of 4%PVA and 7%PVP；2. the PDMS substrate prepared is soaked in PVA and PVP mixed solution
20min places into dry 1.5h in 80 DEG C of vacuum drying oven；3. it is 2. primary to repeat step；4. being then placed in 100 DEG C of vacuum to dry
Heat fixation 20min in case.5. it is 2. and 4. primary to repeat step, the PDMS substrate of surface hydrophilic is obtained.
(3) prepared by PDMS-AgNWs conductive layer.Compound concentration is the silver nanowires ethanol solution of 5mg/mL, silver nanoparticle line gauge
Lattice are as follows: diameter 90nm, 60 μM of length.In the groove for equably spreading over the surface PDMS, place at room temperature drying for one day.
(4) PDMS-AgNWs-AuNPs silver nanowires/nanogold combination electrode preparation.Using PDMS-AgNWs as work
Electrode immerses 1mg/ml KAuCl4With 0.5mol/L H2SO4Mixed electrolytic solution in, reference electrode be Ag/AgCl electrode, auxiliary
Electrode is platinum filament, carries out potentiostatic electrodeposition using chronoamperometry, carries out permanent electricity using the chronoamperometry of electrochemical workstation
Sink product, deposition current are -0.2V, and sedimentation time is respectively 200s, 400s, 800s, 1600s.Place at room temperature it is drying for one day,
Prepare silver nanowires/nanogold combination electrode.
(5) silver nanowires obtained/nanogold combination electrode is bent 100 times, every time 180 ° of bending.As shown in Fig. 5,
Will respectively deposit 200s, deposition 400s, deposition 800s, deposit 1600s nanogold combination electrode stretch 100 times, electrode it is soft
Toughness keeps good, and uses four probe resistance instrument test resistance values after stretching, and sheet resistance increases in the normal range, illustrates electrode drawing
Stretch rear satisfactory mechanical property.
Embodiment 4
(1) PDMS (dimethyl silicone polymer) substrate makes.Electronic palette software design electrode drawing, and benefit are used first
Drawing is printed into mask plate with optical graving version technique, secondly in clean silicon chip surface spin coating photoresist, masking contains electrode
The mask plate of figure, is finally exposed and develops, and obtains silicon wafer template.It places it in batch cultur ware；It pours on it
Infuse the PDMS mixed solution that mass ratio is 10:1；It places into negative pressure in vacuum desiccator and pumps bubble in PDMS mixed solution,
Used time 2h；The 1h of being heating and curing is put into 80 DEG C of constant temperature oven after taking-up；Ready-made substrate is handled with 3M adhesive tape and removes surface
The dust of attachment is then placed in UV ozone cleaning machine and cleans 10min, obtains the PDMS substrate with fixed shaped recesses.
(2) PDMS hydrophilic layer is modified.Reference literature simultaneously does some improvement, the specific steps are as follows: 1. prepares mass percent
For the water mixed solution of 4%PVA and 7%PVP；2. the PDMS substrate prepared is soaked in PVA and PVP mixed solution
20min places into dry 1.5h in 80 DEG C of vacuum drying oven；3. it is 2. primary to repeat step；4. being then placed in 100 DEG C of vacuum to dry
Heat fixation 20min in case.5. it is 2. and 4. primary to repeat step, the PDMS substrate of surface hydrophilic is obtained.
(3) prepared by PDMS-AgNWs conductive layer.Compound concentration is the silver nanowires ethanol solution of 5mg/mL, silver nanoparticle line gauge
Lattice are as follows: diameter 90nm, 60 μM of length.In the groove for equably spreading over the surface PDMS, place at room temperature drying for one day.
(4) PDMS-AgNWs-AuNPs silver nanowires/nanogold combination electrode preparation.Using PDMS-AgNWs as work
Electrode immerses 1mg/ml KAuCl4With 0.5mol/L H2SO4Mixed electrolytic solution in, reference electrode be Ag/AgCl electrode, auxiliary
Electrode is platinum filament, carries out potentiostatic electrodeposition using chronoamperometry, carries out permanent electricity using the chronoamperometry of electrochemical workstation
Sink product, deposition current are -0.2V, and sedimentation time is respectively 200s, 400s, 800s, 1600s.Place at room temperature it is drying for one day,
Prepare silver nanowires/nanogold combination electrode.
(5) silver nanowires obtained/nanogold combination electrode is bent 500 times, each bending angle is 180 °.Such as attached drawing
Shown in 6, combination electrode bending 100 times for 200s being deposited respectively, deposition 400s, 800s is deposited, deposit 1600s nanogold, electricity
The flexibility of pole keeps good, and with four probe resistance instrument test resistance values after bending, sheet resistance increases in the normal range, explanation
Satisfactory mechanical property after electrode bending.
Flexibility silver nanowires/nanogold combination electrode prepared by the present invention, has the characteristics that low resistance, high-mechanical property,
Resistance range: 0.5 Ω sq-1~11 Ω sq-1, the resistance range after bending 500 times: 0.9 Ω sq-1~16 Ω sq-1, stretch 100 times
Resistance range afterwards: 0.8 Ω sq-1~10 Ω sq-1。
Flexible silver nanowires/nanogold combination electrode performance prepared by the method for the present invention is in a leading position in the same industry
Level, electronic component miniaturization and it is integrated in have a good application prospect.
Claims (6)
1. a kind of silver nanowires based on PDMS/nanogold combination electrode, which is characterized in that the silver nanoparticle based on PDMS
Line/nanogold combination electrode includes: that PDMS is substrate, and silver nanowires is conductive layer, and nanogold particle is electrochemical deposition layer, institute
Nanogold particle is stated to be deposited in silver nanowires.
2. a kind of method for preparing the silver nanowires based on PDMS/nanogold combination electrode, method includes the following steps:
S1: in the PDMS monomer that the silicon wafer template upper mass ratio obtained by photolithography method is 1:1-20:1 and cause liquid mixing
Solution obtains the PDMS substrate of fixed shaped recesses after heated solidification；
S2: the mixed solution for the PVP that the PVA and mass concentration that configuration quality concentration is 0.1%-10% are 0.1%-10%, it will
The PDMS substrate prepared in S1 is soaked in PVA and PVP mixed solution, after heated solidification, obtains the PDMS of surface hydrophilic
Substrate；
S3: the silver nanowires ethanol solution that concentration is 0.01-10mg/mL is equably spread in the groove on the surface PDMS, is obtained
To PDMS-AgNWs conductive layer, the silver nanowires length 50-200nm, diameter 30-100nm；
S4: 0.1~5mg/mL KAuCl is immersed using PDMS-AgNWs as working electrode4With 0.1~1mol/L H2SO4Mixing
In electrolyte, reference electrode is Ag/AgCl electrode, and auxiliary electrode is platinum filament, carries out potentiostatic electrodeposition using chronoamperometry, sinks
Product electric current is -0.3~-3mA, 10~1600s of sedimentation time.It is compound to obtain PDMS-AgNWs-AuNPs silver nanowires/nanogold
Electrode.
3. a kind of method for preparing the silver nanowires based on PDMS/nanogold combination electrode as claimed in claim 2, feature
It is, in step sl, the monomer of the PDMS mixed liquor being cast in silicon wafer template and the mass ratio for causing liquid are 10:1.
4. a kind of method for preparing the silver nanowires based on PDMS/nanogold combination electrode as claimed in claim 2, feature
It is, in step sl, the step of pumping the bubble in PDMS mixed solution by negative pressure is needed before heat-curing step,
The step of cleaning by UV ozone is needed after heat-curing step.
5. a kind of method for preparing the silver nanowires based on PDMS/nanogold combination electrode as claimed in claim 2, feature
It is, in step s 2, in the mixed liquor of the PVA and PVP, the concentration that PVA concentration is 4%, PVP is 7%.
6. a kind of method for preparing the silver nanowires based on PDMS/nanogold combination electrode as claimed in claim 2, feature
It is, in step s3, the concentration of the silver nanowires ethanol solution is 5mg/mL.
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| CN113013421A (en) * | 2019-12-19 | 2021-06-22 | 大连大学 | Preparation method and application of PDMS-based silver nanowire/nanogold/nano-nickel composite electrode |
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