CN109298043A - A kind of method of flexible silver nanowires of the application based on PDMS/nanogold combination electrode detection nitrite - Google Patents
A kind of method of flexible silver nanowires of the application based on PDMS/nanogold combination electrode detection nitrite Download PDFInfo
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- CN109298043A CN109298043A CN201811239331.5A CN201811239331A CN109298043A CN 109298043 A CN109298043 A CN 109298043A CN 201811239331 A CN201811239331 A CN 201811239331A CN 109298043 A CN109298043 A CN 109298043A
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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
A kind of flexible silver nanowires/nanogold combination electrode detection nitrite method the present invention relates to application based on PDMS.Using AuNPs/AgNWs/PDMS flexible electrode as working electrode, Ag/AgCl electrode is reference electrode, platinum filament is auxiliary electrode group into three-electrode system, the three-electrode system is placed in nitrite prepare liquid and supporting electrolyte, initial potential is set as 1v, runing time 2000s, sampling interval 0.1s, it records concentration range and is the ampere time graph of 4~3199 μM of mmol/L nitrite, and fit standard curve.It is an object of that present invention to provide a kind of pair of nitrite selectivity with higher, higher sensitivity, and are easier the electrochemical methods of operation.
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
Application of the combination electrode (AuNPs/AgNWs/PDMS electrode) in nitrous nitrification.
Background technique
Nitrite is a kind of industrial salt, has application in many fields, such as: food industry, dyeing industry.And
Nitrite is also widely present in the environment, such as sanitary sewage, industrial wastewater.Existing relevant report confirmation, nitrite one
The typical inorganic pollution of kind, to human health nocuousness.It will lead to cancer or anemia etc. after human body excess intake nitrite
Disease.Since nitrite is very unstable in the environment, and still there is very big defect for the detection of nitrite at present,
Such as: detection device is huge, and valuableness is not suitable for on-site test；It is complicated for operation that time-consuming.Therefore it develops a kind of quick, sensitive, just
The detection method taken is most important.And Electrochemical Detection can exactly realize these demands.Electrochemical method is that one kind passes through electrode
Chemical signal of the determinand in solution when reacting be converted to the detection method of electric signal, this method not only device
Simply, at low cost, easy of integrationization, but also have many advantages, such as that highly sensitive, detection is quick, be currently used detection method it
One.Importantly, examinations may be implemented in electrochemical method.
Summary of the invention
The purpose of the present invention is to provide a kind of pair of nitrite selectivity with higher, higher sensitivity, and compare
It is easier to the electrochemical methods of operation.The present invention with dimethyl silicone polymer (PDMS) be flexible substrates, with polyvinyl alcohol with
Glycerine mixed solution is in its surface modification hydrophilic surface layer, one layer of silver nanowires conductive layer of even spread on hydrophilic decorative layer,
And nanogold particle is deposited using the method for electrochemical deposition on the conductive layer.A kind of measurement nitrous acid is established on this basis
The novel analysis method of salt.
To achieve the above object, the technical solution adopted by the present invention are as follows:
Using AuNPs/AgNWs/PDMS flexible electrode as working electrode, Ag/AgCl electrode is reference electrode, and platinum filament is auxiliary
Electrode forms three-electrode system, which is placed in nitrite prepare liquid and supporting electrolyte, sets initial electricity
Position is 1v, runing time 2000s, sampling interval 0.1s, and record concentration range is 4~3199 μM of mmol/L nitrite
Ampere time graph, and fit standard curve.
Further, the supporting electrolyte contains 0.1mol/L Na2SO4Solution.
Further, the flexible silver nanowires/nanogold combination electrode based on PDMS includes: to use PDMS for base
Bottom, silver nanowires are conductive layer, and nanogold particle is electrochemical deposition layer, and the nanogold particle is deposited in silver nanowires.
The present invention is by the good electric conductivity of silver nanowires and the excellent selectivity of nanogold particle；High catalytic property and chemistry
Inertia combines, and a kind of pair of nitrite, which is prepared, has highly sensitive electrode, and electrochemical analysis method operation letter
It is single, detection time is short, accuracy and high sensitivity, can be widely applied to actual sample measurement.
Detailed description of the invention
Attached drawing 1 is the silver nanowires based on PDMS/nanogold combination electrode surface topography map.
Attached drawing 2 is nitrite prepare liquid and blank solution cyclic voltammetry curve comparison diagram.
Attached drawing 3 is the time-optimized figure of deposition gold.
Attached drawing 4 is scanning circle number comparison diagram.
Attached drawing 5 is AuNPs/AgNWs/PDMS flexible electrode activation figure.
Attached drawing 6 is activation comparison diagram.
Attached drawing 7 is pH value of solution optimization figure.
Attached drawing 8 is that current-vs-time method surveys nitrite response range curve.
Attached drawing 9 is the standard curve of various concentration nitrite.
Specific embodiment
Further description of the technical solution of the present invention in the following with reference to the drawings and specific embodiments, but the present invention not with
Any form constrained is in embodiment content.Experimental method described in embodiment is conventional method unless otherwise specified；Such as without spy
Different explanation, the experiment reagent and material, commercially obtain.
Following embodiment AuNPs/AgNWs/PDMS flexible electrodes the preparation method comprises the following steps:
PDMS substrate is made using photoetching technique.In clean silicon chip surface spin coating photoresist, masking contains electrode pattern
Mask plate, be finally exposed and develop, obtain silicon wafer template.Silicon wafer template is placed in batch cultur ware, matter is poured
Amount is than the PDMS mixed solution for 10:1；It places into negative pressure in vacuum desiccator and pumps bubble in PDMS mixed solution, used time
2h；It is put into 80 DEG C of constant temperature oven the 1h that is heating and curing after taking-up, and is cut into 12 electrode base sheets；By ready-made electrode base sheet
The dust that surface attachment is removed with adhesive tape (being purchased from Minnesota Mining and Manufacturing Company) processing, is then placed in UV ozone cleaning machine and cleans
2min obtains the PDMS substrate with fixed shaped recesses.
The modification of PDMS substrate surface hydrophilic layer.Specific step is as follows: (1) preparing mass percent is 4%PVA and 7%PVP
Mixed aqueous solution；(2) the PDMS substrate prepared is soaked in 20min in PVA and PVP mixed solution, places into 60 DEG C
Dry 2h in vacuum drying oven；(3) it is primary that step (2) are repeated；(4) PDMS substrate is put into heat fixation in 100 DEG C of vacuum drying oven
20min；(5) step (2), (4) are repeated once, obtains the PDMS substrate of surface hydrophilic layer modification.
Electrode preparation.Dehydrated alcohol is mixed by the volume ratio of 9:1 as solvent with water, compound concentration is the silver of 5mg/mL
Nanowire solution in the groove that silver nanowires solution is equably spread over to PDMS substrate surface, places dry one at room temperature
More than it, that is, AgNWs/PDMS ductile electrode is prepared, then, using AgNWs/PDMS as working electrode, Ag/AgCl electrode is ginseng
Than electrode, platinum filament is auxiliary electrode, immerses 1mg/ml KAuCl4With 0.5mol/L H2SO4Mixed electrolytic solution in, in -0.2V
Under potential condition, AuNPs/AgNWs/PDMS is obtained in the deposition that its surface carries out nanogold particle using electrochemical workstation,
It places at room temperature drying for one day.
As shown in Figure 1, silver nanowires is evenly distributed on flexible electrode surface, overlap joint is close；Gold nano grain size and point
Cloth is uniform.Illustrate that the novel electrode is functional.
1 nitrite solution of embodiment and blank solution cyclic voltammetry curve compare
Firstly, three-electrode system is placed in 0.1mol/L Na2SO4In solution, using cyclic voltammetry, in 0.2~1.4V
Potential range in be scanned, record the cyclic voltammetry curve of blank solution；Then, by three-electrode system be placed in containing
0.1mol/L Na2SO4Solution as in the nitrite prepare liquid of the 20mmol/L of supporting electrolyte utilize cyclic voltammetry,
It is scanned in the potential range of 0.2~1.4V, records the cyclic voltammetry curve of nitrite.As shown in Fig. 2.
The AuNPs/AgNWs/PDMS electrode of the not synsedimentary golden time of embodiment 2 responds the cyclic voltammetric of nitrite
It is 200s that the golden time, which will successively be deposited,；400s；800s；1600s；The AuNPs/AgNWs/PDMS electrode of 3200s is set
In contain 0.1mol/L Na2SO4Solution waits for that nitrite is surveyed in liquid as the 20mmol/L of supporting electrolyte, utilizes cyclic voltammetric
Method is scanned in the potential range of 0.2~1.4V, records the nitrite response cycle volt of the golden time electrode of not synsedimentary
Pacify curve.The optimal deposition gold time is 1600s, because its peak current highest, oxidation peak current reach 2.84mA, and oxidizing potential
The electrode of more other sedimentation times is lower, only 1.02V, illustrates electrode prepared by the sedimentation time, for nitrite
Oxidation reaction is more easier to carry out.As shown in Fig. 3.
The influence of the scanning several pairs of nitrite test results of circle of embodiment 3
Three-electrode system is placed in containing 0.1mol/L Na2SO4Nitrous of the solution as the 10mmol/L of supporting electrolyte
Cyclic voltammetry is utilized in hydrochlorate prepare liquid, is scanned in the potential range of 0.2~1.4V, respectively writing scan 1-4 circle
The cyclic voltammetry curve of nitrite.With the increase of scanning circle number, cyclic voltammetry curve becomes more and more smooth and stablizes,
After sweeping to third circle, the oxidation peak peak type of nitrite is more preferable, and after scanning the 4th circle again, spike potential and peak current almost without
Variation, therefore following experiment is all using the cyclic voltammetry curve after three circle of scanning.As shown in Fig. 4.
4 working electrode of embodiment activates the influence to nitrite test result
Firstly, using AuNPs/AgNWs/PDMS electrode as working electrode, Ag/AgCl makees as reference electrode, platinum electrode
For to electrode, this three electrode is placed in containing 0.05mol/LH2SO4In solution, it is activated using cyclic voltammetry ,-
It is scanned in the potential range of 1~1V.Electrode activation figure is as shown in Fig. 5.
Three-electrode system is placed in containing 0.1mol/L Na later2SO415mmol/L of the solution as supporting electrolyte
Cyclic voltammetry is utilized in nitrite prepare liquid, is scanned in the potential range of 0.2~1.4V, is recorded nitrite
Cyclic voltammetry curve and unactivated test result compare.As shown in Fig. 6.Dotted line is nitrite cyclic voltammetric song after activation
Line, it is found that its spike potential is shuffled, and electrode is sensitiveer for the response of nitrite after this shows activation.
Influence of 5 pH value of solution of embodiment to test result
Three-electrode system is respectively placed in pH value and contains 0.1mol/L Na for 4-82SO4Solution is as supporting electrolyte
Cyclic voltammetry is utilized in the nitrite prepare liquid of 12mmol/L, is scanned in the potential range of 0.2~1.4V, respectively
Record the cyclic voltammetry curve of nitrite under different ph values.By comparing cyclic voltammetric testing result, it is found that when ph is 4, inspection
The oxidation peak current highest for surveying nitrite, reaches 2.06mA.Therefore this experiment Na2SO4Solution ph optimum results are 4, and experiment is all
Using the Na of ph=42SO4Solution is as supporting electrolyte.As shown in Fig. 7.
6 amperes-Time Method of embodiment surveys nitrite response range
Three-electrode system is placed in containing 0.1mol/L Na2SO4In solution, it is real that ampere is carried out under continuous magnetic agitation
It tests.Using current-vs-time method, setting initial potential is 1.0V, runing time 2000s, after running 100s, every 60s to
10 μ L nitrite solutions, 35 wherein 10mmol/L nitrite solution 5 times in total, 30mmol/L nitrous acid are added in solution
Salting liquid 5 times, 50mmol/L nitrite solution 5 times, 100mmol/L nitrite solution 5 times, 300mmol/L nitrite
Solution 6 times, 500mmol/L nitrite solution 6 times, 1000mmol/L nitrite solution 3 times.Record current-time graph.
As shown in Fig. 8.After nitrite is added every time, response current can change rapidly.Steady-state current is dense with nitrite
Degree is in good linear relationship at 4~3199 μM.As shown in Fig. 8
Using origin software, standard curve is made, which is y=8.36348 × 10-6+ 0.42131x is related
Coefficient is 0.99787.Detection is limited to 2.284 μM.As shown in Fig. 9.
The preferable specific embodiment of the above, only the invention, but the protection scope of the invention is not
It is confined to this, anyone 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 scope it
It is interior.
Claims (3)
1. a kind of flexible silver nanowires of application based on PDMS/nanogold combination electrode detection nitrite method, feature
It is, using AuNPs/AgNWs/PDMS flexible electrode as working electrode, Ag/AgCl electrode is reference electrode, and platinum filament is auxiliary electricity
Pole forms three-electrode system, which is placed in nitrite prepare liquid and supporting electrolyte, sets initial potential
For 1v, runing time 2000s, sampling interval 0.1s, recording concentration range is 4~3199 μM of mmol/L nitrite
Ampere time graph, and fit standard curve.
2. a kind of flexible silver nanowires of the application based on PDMS/nanogold combination electrode as described in claim 1 detects nitrous
The method of hydrochlorate, which is characterized in that the supporting electrolyte contains 0.1mol/L Na2SO4Solution.
3. a kind of flexible silver nanowires of the application based on PDMS/nanogold combination electrode as described in claim 1 detects nitrous
The method of hydrochlorate, which is characterized in that the flexible silver nanowires/nanogold combination electrode based on PDMS includes: use
PDMS is substrate, and silver nanowires is conductive layer, and nanogold particle is electrochemical deposition layer, and the nanogold particle is deposited on Yin Na
On rice noodles.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112986350A (en) * | 2019-12-16 | 2021-06-18 | 大连大学 | Method for detecting nitrite by using AuNPs/NiNFs/ITO electrode |
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| CN101966594A (en) * | 2010-10-18 | 2011-02-09 | 上海市七宝中学 | Electro-deposition gold nanoparticles, preparation method and application thereof |
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| CN101966594A (en) * | 2010-10-18 | 2011-02-09 | 上海市七宝中学 | Electro-deposition gold nanoparticles, preparation method and application thereof |
| KR20150134773A (en) * | 2014-05-23 | 2015-12-02 | 국립대학법인 울산과학기술대학교 산학협력단 | Flexible electrode and manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112986350B (en) * | 2019-12-16 | 2022-05-13 | 大连大学 | Method for detecting nitrite by using AuNPs/NiNFs/ITO electrode |
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