CN108152348A - A kind of preparation method and application that can be used repeatedly the miniature software Ag/AgCl electrodes based on PDMS - Google Patents
A kind of preparation method and application that can be used repeatedly the miniature software Ag/AgCl electrodes based on PDMS Download PDFInfo
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- CN108152348A CN108152348A CN201711401790.4A CN201711401790A CN108152348A CN 108152348 A CN108152348 A CN 108152348A CN 201711401790 A CN201711401790 A CN 201711401790A CN 108152348 A CN108152348 A CN 108152348A
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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
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
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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
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
Abstract
The present invention relates to electrochemical electrode preparation fields, and in particular to a kind of preparation method and application that can be used repeatedly the miniature software Ag/AgCl electrodes based on PDMS.The present invention carries out surface hydrophilic modification using flexible PDMS as electrode base materials, by electrode base materials, then even spread nano silver wire, then is soaked in aoxidize in NaClO solution and Ag/AgCl electrodes are made.It is used as using Ag/AgCl electrodes of the present invention and shows good job stability and sensitivity with reference to electrode, and operating potential will be less than traditional electrode, sustainable work 1 hour or more.Electrode of the present invention can repeatedly use, material non-toxic and biocompatibility is good is widely used in micro sprue system, which, which can develop, is used as biological body sensor.
Description
Technical field
The present invention relates to electrochemical technology fields, and in particular to a kind of reusable micro-fluidic electrode based on PDMS
The preparation and application of Ag/AgCl electrodes.
Background technology
In the research of recent electrochemistry, the research of miniature reference electrodes has been a concern.Ag/AgCl electrodes are applications
One of most wide reference electrode, since it has many advantages, such as the operation is stable, preparation process is simple and without security risk, is used
It will be of great significance in biological monitoring and micro-fluidic detection.Miniature Ag/AgCl electrodes are prepared at present mainly uses silk screen
Printing technology, using PET as electrode base material, silver paste is printed onto on base material as conductor paste and makes electrode by silver ink.
This method although it is easy to operate can mass industrial production, but electrode surface state is difficult to control, electrode performance difference between batch
Big job insecurity.And the technology is difficult to design, regulates and controls electrode size and shape；Waste a large amount of material.Due to electrode base
The easy temperature distortions of material PET, and poor biocompatibility is not used to high temperature and biological in-vivo monitoring.Silva later[1]Have studied spray
Ink printing Ag/AgCl electrodes, the advantage of this method be electrode shape can designed, designed and regulation and control size, and job stability is excellent
It is different and can be printed on a variety of base materials, it is cost-effective etc..But electrode surface Ag/AgCl layers after oxidation of inkjet printing Ag electrodes
It easily comes off, causes sustainable stable work time only within 30 minutes.And Rius-Ruiz[2]It prepares carbon nano tube modified
Ag/AgCl reference electrodes after 3min just can steady operation, sensitivity is low.
[1] Silva, D.；Miserere, S.；Kubota, T., Simple On-Plastic/Paper Inkjet-
Printed Solid-StateAg/AgCl Pseudoreference Electrode, Anal.Chem.2014,86,10531-
10534
[2] F.XavierRius-Ruiz, DiegoBejarano-Nosas, Blondeau, P., Riu, J.,
Disposable Planar Reference Electrode Based on Carbon Nanotubes and
Polyacrylate Membrane, Anal.Chem.2011,83,5783-5788.
Invention content
It is an object of the invention to prepare a kind of miniature software Ag/AgCl electrodes that can be used repeatedly, silica gel can be passed through
Photoetching technique regulates and controls electrode size and design electrode shape.The present invention is for the first time using PDMS as the base material with reference to electrode, using silver
Working lining of the nano wire as electrode prepares Ag/AgCl electrodes with chemical oxidization method.
To achieve the above object, the technical solution adopted by the present invention is：It, will be electric using flexible PDMS as electrode base materials
Pole base material, which is soaked in the decorating liquid of 5wt%Gly and 2wt%PVA compositions, carries out surface hydrophilic modification, then in electrode base
Bottom material surface even spread nano silver wire after 60 DEG C dry 2h, then is soaked in aoxidize in NaClO solution and Ag/AgCl is made
Electrode.
The application of above-mentioned Ag/AgCl electrodes is claimed in another object of the present invention, is working electrode by glass-carbon electrode,
Ag/AgCl is reference electrode, platinum filament be assist electrode group into three-electrode system.The three-electrode system is placed in KCl (10- 4Mol/L it) works in solution.
The present invention has low cost, recyclable recycling, bio-compatible for the first time using PDMS as the base material with reference to electrode
The advantages that property is good, and it is better than PVC and PET by electrode of the substrate job stability of PDMS.The present invention can pass through silicon chip light
The mode for carving silica gel designs electrode base material mold, electrode is made not limited by shape size, application is more extensive.Nanometer is used for the first time
Silver wire chemical method prepares Ag/AgCl electrode working linings, which prepares existing fabulous job stability (the △ E of the electrode obtained<3mv)
And sensitivity (t<20s), electrode potential will be less than the survey that traditional commerce electrode about 0.263v has greatly widened reference electrode
Measure section.Sustainable more than the work 1h of reference electrode is prepared, and be used multiple times using the present invention, it is accumulative to be using maximum duration
90min.Nano silver wire electrode of the present invention needs nitrogen charging gas shielded after NaClO oxidations, and electrode carries protective device convenient for preserving,
It is protected from light in the case of the protection of no nanometer that preserve 1 year or more can normal use.Electrode of the present invention can repeatedly use, material without
Poison and biocompatibility is good is widely used in micro sprue system, which, which can develop, is used as biological body sensor.
Description of the drawings
Fig. 1 is the selection figure of nano silver wire anodizing agent concentration；
Fig. 2 optimizes oxidization time figure for chronoptentiometry；
Fig. 3 Ag/AgCl electrodes of the present invention and traditional commerce electrode work contrast test figure；
Fig. 4 is length nano silver wire and the comparison time-measuring electric potential curve graph for depositing nano silver；
Fig. 5 is PET；PVA；The comparison timing electricity of Ag/AgCl reference electrodes is made respectively as the base material of reference electrode by PDM
Position curve graph；
Fig. 6 is the sustainable time time-measuring electric potential curve graph of Ag/AgCl reference electrodes work；
Fig. 7 lays in stability test time-measuring electric potential curve graph for electrode；
After Fig. 8 is stands for 24 hours, three-electrode system electrode performance test time-measuring electric potential in KCl supporting electrolyte solutions is bent
Line chart；
Fig. 9 replaces supporting electrolyte solution KCl, electrode performance test time-measuring electric potential for work 30min and after placing for 24 hours
Curve graph；
Figure 10 is the 60min and after placing for 24 hours of having worked, and supporting electrolyte solution KCl is replaced, during electrode performance tester
Potential curve figure；
Figure 11 is the 90min and after placing for 24 hours of having worked, and supporting electrolyte solution KCl is replaced, during electrode performance tester
Potential curve figure；
After Figure 12 is places for 24 hours, it is changed without supporting electrolyte solution KCl, potential curve figure during electrode performance tester；
It after Figure 13 is work 30min, and places for 24 hours, is changed without supporting electrolyte solution KCl, during electrode performance tester
Potential curve figure；
Figure 14 cyclic voltammetry curves, wherein making reference electrode with nano wire Ag/AgCl；
Figure 15 makes reference electrode schematic diagram by oneself.
Specific embodiment
Technical scheme of the present invention is described in detail with reference to the accompanying drawings and examples.Wherein nano silver wire is purchased from Nanjing elder generation
Rich Nono-material Science ＆ Technology Ltd..
Cure 2h at 100 DEG C after PDMS is mixed by PDMS and the 10wt% curing agent of 90wt% in following embodiments to prepare
It obtains.
Embodiment 1 prepares Ag/AgCl reference electrodes：
1. the preparation of electrode base material mold：
(1) prepare two roasting glue machines be adjusted to respectively 65 DEG C and 200 DEG C it is spare, new silicon chip is taken to be blown clean with nitrogen and is placed on heat
On plate, 5min is heated on 200 DEG C of roasting glue machines.Then silicon chip is cooled down in room temperature.
(2) center of silicon chip is aligned placement with the center of spin coating instrument turntable, photoresist is added dropwise in silicon chip center, is being added dropwise
During cannot generate bubble, then silicon chip is placed on 65 DEG C of roasting glue machines by the whirl coating 20s at a slow speed under the rotating speed of 500r/min
5min is heated, 20min is heated at 95 DEG C, silicon chip cools down 10min in room temperature after heating.
(3) silicon chip is placed in mask plate, is exposed under the ultraviolet exposure machine of wavelength 280nm, the silicon chip after exposure is placed in
On hot plate, 5min is heated with 65 DEG C of roasting glue machines, then heats 11min on 95 DEG C of roasting glue machines.Finally it is cooled to room temperature.
(4) silicon chip from hot plate is removed, be positioned in glass culture dish, add in developer solution, constantly slight concussion, until
Figure is high-visible.Extra developer solution is rinsed out with acetone and deionized water, room temperature is dried.
2. the preparation of electrode working lining chip：
It is poured in electrode base material mold after being mixed by PDMS and the 10wt% silane coupling agent of 90wt%, it is solid at 100 DEG C
Change 2h, flexibility PDMS is made.Then hydrophilic modification flexibility PDMS, decorating liquid are made of 5wt% (Gly) and 2wt% (PVA), will
60 DEG C of drying 2h of taking-up are operated three times repeatedly after flexible PDMS is soaked in decorating liquid 20min, last even spread nano silver wire, and 60
DEG C drying 2h after carry out anodizing processing again, be immersed in NaClO (20mg/mol), 60 DEG C after finally being rinsed with deionized water
Drying 2h just obtains Ag/AgCl reference electrodes.
The making of 3.Ag/AgCl electrode PDMS hollow shells and PDMS films：
The PDMS hollow shells of electrode are prepared using the preparation method identical with flexible PDMS, which is hollow structure inside,
For storing supporting electrolyte kcl.Then configuration glue coheres PDMS hollow shells and Ag/AgCl electrodes, and glue can be by
PDMS and the 10wt% curing agent (such as silane coupling agent) of 90wt% is mixed to prepare.
PDMS films are the containment device of electrode top layer, and preparation concrete operations are identical with PDMS hollow shells, last preparing
It needs to be punched with card punch.Electrode schematic diagram is shown in attached drawing 15.
Embodiment 2
Ag/AgCl electrodes prepared by embodiment 1 are reference electrode, and glass-carbon electrode is working electrode, and platinum filament is auxiliary electricity
Pole forms three-electrode system.
The pretreatment of glass-carbon electrode：Glass-carbon electrode is polished and is activated, uses the different Al of grain size203Powder, from large to small,
It is placed on deerskin and is added dropwise less than deionized water polishing electrode.
Electrode test is carried out using the three-electrode system of the present embodiment：
The electrode is placed in PBS (10x) buffer solution by the three-electrode system, under three-electrode system, using timing
Potentiometry sets cathode current as 2 μ A, and anode current is 2 μ A, and cathode span 2s, the anode time is 600s, and initial polarity is
Anode, 0.01s, hop count 2 are divided between data storage, and polarity of electrode switching mode is the time.Time-measuring electric potential curve is shown in Fig. 3.
Electrode work contrast test figure (a chronoptentiometries as shown in Figure 3；B testing impedances).By with traditional commerce electrode
Comparison understands the Ag/AgCl nano wires prepared since test to electrode the operation is stable, embodiment 1 by chronoptentiometry analysis
Electrode only used time about 20s, and then used time nearly 100s just can steady operation for business electrode.Ag/AgCl nano line electrodes are due to nanometer
Structure causes electrode potential to reduce, lower than traditional commerce reference electrode current potential about 26.3%, having widened the measurement of reference electrode makes
With range and accuracy.Comprehensive impedance test understands Ag/AgCl nano line electrodes in its electron transmission ability of low frequency range higher than biography
System business electrode.Ag/AgCl nano line electrodes △ E after 340s<3mv.
Embodiment 3
Three-electrode system is working electrode by glass-carbon electrode, and nano wire Ag/AgCl prepared by embodiment 1 is reference electrode,
Platinum filament for auxiliary electrode group into.
The pretreatment of glass-carbon electrode：Glass-carbon electrode is polished and is activated, uses the different Al of grain size203Powder, from large to small,
It is placed on deerskin and is added dropwise less than deionized water polishing electrode.
Electrode test is carried out using the three-electrode system of the present embodiment：
The electrode is placed in the potassium ferricyanide (10 by the three-electrode system-6Mol/L it) in solution, under three-electrode system, adopts
With cyclic voltammetry, it is -0.8 to 1.0v to set scanning potential range, sweeps speed as 0.1v/s, the number of turns is enclosed for 1, cyclic voltammetry curve
See Figure 15.
The reference electrode Ag/AgCl of the present invention technological parameters prepared are optimized, test result is as follows.
Attached drawing 1 is the selection figure of nanometer Ag line electrode oxidant concentration.As shown in Figure 1, figure a is does not aoxidize Ag electrodes surface layer
Nano-silver thread structure, figure b is is immersed in oxidant NaClO (40mg/mol) Ag/AgCl structures after 60s, and figure c is is immersed in oxygen
Ag/AgCl structures after 60s in agent NaClO (20mg/mol).Scheme d to detect for electrode surface layer atomic spectrum, be aoxidized by comparing
The atomic spectrum on front and rear electrode surface layer shows to have generated AgCl after oxidation.Scheme e, f is respectively various concentration oxidant impedance
Analysis and chronopotentiogram.To sum up analysis can determine a concentration of 20mg/mol of oxidant NaClO, the work of Ag/AgCl reference electrodes
Performance is best.
Attached drawing 2 optimizes oxidization time figure for chronoptentiometry.Three-electrode system is placed in KCl (10-4Mol/L) in solution,
Using chronoptentiometry, cathode current is set as 2 μ A, and anode current is 2 μ A, and cathode span 2s, the anode time is 600s, just
Beginning polarity is anode, and 0.01s, hop count 2 are divided between data storage, and polarity of electrode switching mode is the time.Finally determine reference
Electrode Ag/AgCl optimum oxidation times are 60s.
Comparison of the attached drawing 4 for length nano silver wire and deposition nano silver, is detected using chronoptentiometry, finally proves short silver
Nano wire (60 μm of length, diameter 90nm) electrode performance is best.Deposit the electrode potential highest of nano-Ag particles but its work
Stability is bad, illustrates that silver nano-grain is unevenly distributed on nano-silver thread, causes conduction electronics unstable.Short nano-silver thread
Electrode operating potential is higher than long nano-silver thread electrode and good operating stability, so short nano silver wire is as electrode working layer
Most preferably.
The comparison of Ag/AgCl reference electrodes is made for PET, PVA, PDMS respectively as the base material of reference electrode for attached drawing 5, adopts
It is detected with chronoptentiometry, finally proves that PDMS is best as the electrode of the substrate performance of reference electrode.
Attached drawing 6 is the service life for probing into Ag/AgCl reference electrodes, using chronoptentiometry, the electricity prepared with embodiment 1
Pole is tested as reference electrode, PBS buffer solution as electrode working environment.Prove that self-control Ag/AgCl reference electrodes can be steady
Surely work more than 1h.
Attached drawing 7 lays in stability test for electrode, it can be found that after continuously placing 15 there is significantly current potential after its stabilization
Decline, finally prove that self-made electrode is easily aoxidized, so as to which current potential be caused to decline so that electrode performance is unstable, so electrode needs
It to be preserved in nitrogen.
Using glass-carbon electrode as working electrode, nano wire Ag/AgCl prepared by embodiment 1 is reference electrode, and platinum filament is auxiliary
Electrode forms three-electrode system, after placing for 24 hours, replaces supporting electrolyte solution KCl (10-4Mol/L electrode performances are tested, and are used
Chronoptentiometry is tested, and each length of testing speech is 10min, is tested altogether three times.Test result is as shown in figure 8, electrode reproducibility is excellent
It is different.Work 10min after with work 20min after △ E<5mv, work 20min after with work 30min after △ E<6mv.
By above-mentioned electrode work 30min and after placing for 24 hours, the test of supporting electrolyte solution electrode performance is replaced, using meter
When potentiometry test, each length of testing speech be 10min, altogether test three times.Test result is as shown in figure 9, electric after the 20min that works
Position occurs declining about 2.4%.
Above-mentioned electrode has been worked 60min and after placing for 24 hours, the test of supporting electrolyte solution electrode performance has been replaced, adopts
It is tested with chronoptentiometry, each length of testing speech is 10min, is tested altogether three times.Test result is as shown in Figure 10, it can be seen that three
Time-measuring electric potential curve is stablized obtained by secondary test, therefore is believed that electrode still steady operation.
After attached drawing 11 is work 90min, the test of supporting electrolyte solution electrode performance is replaced.It is surveyed using chronoptentiometry
Examination, electrode potential significantly fluctuates, therefore thinks electrode failure.
After attached drawing 12 is places for 24 hours, the test of supporting electrolyte solution electrode performance is changed without, is surveyed using chronoptentiometry
Examination, each length of testing speech are 10min, are tested altogether three times.It can be seen that test gained time-measuring electric potential curve is stablized three times, therefore can recognize
For electrode still steady operation.
It after attached drawing 13 is work 30min, and places for 24 hours, the test of supporting electrolyte solution electrode performance is changed without, using meter
When potentiometry test.Electrode potential significantly occurs fluctuating (i.e. broken line fluctuation occurs in time-measuring electric potential curve), therefore thinks electrode failure.
As shown in figure 14, nano wire Ag/AgCl reference electrodes of the present invention can be normal in redox system occurs
Work.
Claims (7)
1. a kind of preparation method that can be used repeatedly the miniature software Ag/AgCl electrodes based on PDMS, which is characterized in that with soft
Property PDMS as electrode base materials, by electrode base materials be soaked in the decorating liquid of 5wt%Gly and 2wt%PVA compositions into
Row surface hydrophilic is modified, and then in electrode base materials surface even spread nano silver wire, after 60 DEG C dry 2h, then is soaked in
It is aoxidized in NaClO solution and Ag/AgCl electrode working lining chips is made.
2. according to the method described in claim 1, it is characterized in that, the flexible PDMS by 90wt% PDMS and 10wt%
It is poured in electrode base material mold after curing agent mixing, cures 2h at 100 DEG C and be made.
3. according to the method described in claim 2, it is characterized in that, the curing agent is silane coupling agent.
4. according to the method described in claim 1, it is characterized in that, the method for surface hydrophilic modification is：By electrode basement
Material is soaked in the decorating liquid of 5wt%Gly and 2wt%PVA compositions after 20min to take out operates 2-3 repeatedly in 60 DEG C of drying 2h
It is secondary.
5. according to the method described in claim 1, it is characterized in that, the NaClO solution concentrations are 20mg/mol.
6. according to the method described in claim 1, it is characterized in that, the electrode base material mold utilizes silicon chip photoetching silica gel
Prepared by mode.
7. the application of Ag/AgCl electrodes prepared by a kind of method as described in claim 1, which is characterized in that by Ag/AgCl electricity
As reference electrode, glass-carbon electrode is working electrode for pole, and platinum filament is auxiliary electrode, forms three-electrode system.
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Cited By (6)
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| CN109171699A (en) * | 2018-08-27 | 2019-01-11 | 厦门大学 | A kind of silk microneedle electrodes and preparation method thereof |
| CN110146114A (en) * | 2019-05-20 | 2019-08-20 | 河北工业大学 | A kind of flexible array microelectrode preparation method |
| CN112285181A (en) * | 2020-10-23 | 2021-01-29 | 徐州工业职业技术学院 | Preparation method of enzyme sensor for realizing hydrogen peroxide detection |
| CN112967832A (en) * | 2021-02-01 | 2021-06-15 | 天津理工大学 | Flexible comb-shaped semi-dry electrode and preparation method thereof |
| CN113647952A (en) * | 2021-08-18 | 2021-11-16 | 北京航空航天大学 | Flexible dry electrode made of silver/silver chloride nanowires and preparation method thereof |
| WO2023104049A1 (en) * | 2021-12-07 | 2023-06-15 | 深圳先进技术研究院 | Elastic dry electrode, and preparation method therefor and use thereof |
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| CN113647952A (en) * | 2021-08-18 | 2021-11-16 | 北京航空航天大学 | Flexible dry electrode made of silver/silver chloride nanowires and preparation method thereof |
| WO2023104049A1 (en) * | 2021-12-07 | 2023-06-15 | 深圳先进技术研究院 | Elastic dry electrode, and preparation method therefor and use thereof |
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