CN106932453A - A kind of electrode and preparation method thereof and Sensors ＆ Application - Google Patents
A kind of electrode and preparation method thereof and Sensors ＆ Application Download PDFInfo
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- CN106932453A CN106932453A CN201710212663.3A CN201710212663A CN106932453A CN 106932453 A CN106932453 A CN 106932453A CN 201710212663 A CN201710212663 A CN 201710212663A CN 106932453 A CN106932453 A CN 106932453A
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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
- G01N27/36—Glass electrodes
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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 electrode and preparation method thereof and Sensors ＆ Application, it relates generally to field of graphene.The electrode is by setting on electrode matrix the nanometer composite layer being made up of nitrogen-doped graphene silver Jenner's nano composite material so that the chemical property and catalytic performance of the electrode are improved；By simple drop coating method so that preparing the technique of the electrode becomes extremely simple；Cu is applied to by the electrochemical sensor that will include above-mentioned electrode2+Detection in carry out analysis of experiments discovery, it is not only simple to operate and friendly to environment, and the sensitivity with superelevation and non-constant width the range of linearity.Therefore above-mentioned electrode and preparation method thereof and include the Sensors ＆ Application of the electrode and have very big application value.
Description
Technical field
The present invention relates to field of graphene, in particular to a kind of electrode and preparation method thereof and Sensors ＆ Application.
Background technology
Although Graphene only monoatomic layer thickness, used as the carbon material for remaining good crystalline structure, it has solely
(2D) structures, excellent mechanical performance, remarkable chemical property and big specific surface area are tieed up in special 2, and it is in light, electricity, magnetic etc.
Aspect is widely used.
The band structure of Graphene can be adjusted with chemical element doped graphene, changed its electrochemical properties, adjusted it
The band gap width of surface chemical property and change Graphene.In numerous foreign atoms, nitrogen-atoms has preferable atom big
It is small and can form strong covalent bond with carbon containing 5 covalent bonds, be very outstanding chemical doping element, but presently, there are
Problem is much to be showed in terms of catalytic performance and chemical property very not to the nano composite material that nitrating in Graphene is made
Ideal, this is limited by very large its application in terms of catalytic performance and chemical property.
The content of the invention
It is an object of the invention to provide a kind of electrode, it has excellent catalytic performance and chemical property.
Another object of the present invention is to provide a kind of preparation method of electrode, the method preparation process is simple, and can make
It is standby go out the electrode with good chemical property and catalytic performance.
Another object of the present invention is to provide a kind of sensor, it is not only simple to operate and friendly to environment, and with super
Sensitivity high and the range of linearity of non-constant width.
The present invention also provides a kind of sensor in detection Cu2+In application, its can overdelicate quick detection go out Cu2+。
The present invention solves its technical problem to be realized using following technical scheme.
The present invention proposes a kind of electrode, and it includes electrode matrix and is arranged at the nanometer composite layer on electrode matrix surface, its
In, nanometer composite layer is made up of nitrogen-doped graphene-silver Jenner's nano composite material.
The present invention proposes a kind of preparation method of above-mentioned electrode, and it is comprised the following steps：Electrode matrix is thrown successively
After light, washing and drying, by the water-soluble drop-coated of nitrogen-doped graphene-silver Jenner's nano composite material on electrode matrix, and carry out
Naturally dry.
The present invention proposes a kind of sensor, and it includes above-mentioned electrode.
The invention allows for a kind of the sensor in detection Cu2+In application.
Electrode of the embodiment of the present invention and preparation method thereof and the beneficial effect of Sensors ＆ Application are：By in electrode base
The nanometer composite layer that is made up of nitrogen-doped graphene-silver Jenner's nano composite material is set on body so that the chemical property of this electrode and
Catalytic performance is improved；By simple drop coating method so that preparing the technique of the electrode becomes extremely simple；Therefore, wrap
The sensor of above-mentioned electrode is included, it is not only simple to operate and friendly to environment, and the sensitivity with superelevation and non-constant width is linear
Scope, it is used for Cu2+Detection in, show good chemical property and catalytic performance.
Brief description of the drawings
Technical scheme in order to illustrate more clearly the embodiments of the present invention, below will be attached to what is used needed for embodiment
Figure is briefly described, it will be appreciated that the following drawings illustrate only certain embodiments of the present invention, thus be not construed as it is right
The restriction of scope, for those of ordinary skill in the art, on the premise of not paying creative work, can also be according to this
A little accompanying drawings obtain other related accompanying drawings.
Fig. 1 is the sensor in test example with different modifying electrode in the Tris-HCl solution that 0.1mol/L, pH are 7.4
In CV test collection of illustrative plates；
Fig. 2 be test example in sensor under optimum experimental condition, determine Cu2+The DPV figures of concentration, wherein, Fig. 2 (A) table
That show is different Cu2+The DPV figures of concentration, that Fig. 2 (B) is represented is oxidation peak current and Cu2+The linear relationship chart of concentration.
Specific embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below will be in the embodiment of the present invention
Technical scheme be clearly and completely described.Unreceipted actual conditions person, builds according to normal condition or manufacturer in embodiment
The condition of view is carried out.Agents useful for same or the unreceipted production firm person of instrument, are the conventional product that can be obtained by commercially available purchase
Product.
Electrode of the embodiment of the present invention and preparation method thereof and Sensors ＆ Application are specifically described below.
A kind of electrode provided in an embodiment of the present invention, it includes that electrode matrix is answered with the nanometer for being arranged at electrode matrix surface
Layer is closed, wherein it is desired to illustrate, the electrode is mainly used in carrying out electro-chemical test and Cu2+Detection is used, therefore, the present invention
The nanometer composite layer provided in embodiment is made up of nitrogen-doped graphene-silver Jenner's nano composite material.
Further, nitrogen-doped graphene-silver Jenner's nano composite material is by silver nitrate solution, graphene oxide solution, chlorine
It is made after auric acid solution and carbonic acid ammonia hybrid reaction.It should be noted that nitrogen-doped graphene-silver Jenner's nano composite material is specific
Ground preparation process be：After silver nitrate solution and graphene oxide water solution are mixed, then mix with chlorauric acid solution and carbonic acid ammonia
And react.Wherein, the concentration of silver nitrate solution is 0.08-0.12mol/L, and the mass concentration of graphene oxide solution is 0.8-
1.2g/L, the mass percent of the gold chloride in chlorauric acid solution is the nitric acid in 0.8%-1.2%, and silver nitrate solution
The mass ratio of graphene oxide, the gold chloride in chlorauric acid solution and carbonic acid ammonia in silver, graphene oxide water solution is 1.6-
1.8：0.8-1.2：4.8-5.2：490-510.
It is emphasized that above-mentioned carried out for silver nitrate solution, graphene oxide solution, chlorauric acid solution and carbonic acid ammonia
The limitation of amount concentration and mass ratio, primarily to allow between each component sufficiently being reacted, it is ensured that gained nitrogen-doped graphene-
The quality of silver-colored Jenner's nano composite material, in addition, after reaction terminates, in addition it is also necessary to washed successively to products therefrom, precipitated and done
It is dry, you can to obtain nitrogen-doped graphene-silver gold nano composite material powder.
Further, in order to ensure to wash optimum efficiency, washing process carries out multiple centrifuge washing using ultra-pure water, until
Untill the pH of supernatant liquor is 7 or so；In addition, using vacuum drying when being dried, its vacuum drying temperature is 58-62 DEG C,
Drying time is 11-13h, it is preferable that vacuum drying temperature is 60 DEG C, and drying time is 12h, it is emphasized that, using true
Empty drying mode, and the vacuum drying parameter of controller is primarily to allow nitrogen-doped graphene-silver gold nano composite material powder
Not oxidized pollution, so as to maintain its quality stability.
The embodiment of the present invention also proposed the preparation method of above-mentioned electrode, and it is comprised the following steps：
After being polished successively to electrode matrix, washed and being dried, by above-mentioned nitrogen-doped graphene-silver Jenner's nano composite material
Water-soluble drop-coated on electrode matrix, and carry out nature and dry.
Further, after drying naturally, nitrogen-doped graphene-silver Jenner nano composite material of the drop coating on electrode matrix
Form nanometer composite layer.It should be noted that in order to ensure nanometer composite layer chemical property and and electrode matrix combination
Quality, the aqueous solution mass concentration of nitrogen-doped graphene-silver Jenner's nano composite material should be controlled in 0.9-1.1g/L, it is therefore preferable to
1.0g/L, the aqueous solution mass concentration that this is primarily due to nitrogen-doped graphene-silver Jenner's nano composite material is too small, what it was formed
The bond strength of nanometer composite layer is inadequate, and mass concentration is too big, and the nanometer composite layer that it is formed is easy to produce chap again
Split, therefore the bulk strength of nanometer composite layer can be lowered, and also its chemical property also can accordingly weaken, therefore, for drop coating
The aqueous solution mass concentration of the nitrogen-doped graphene-silver Jenner's nano composite material on electrode matrix should give strict control.
Further, in order to lift the total quality of electrode, it is preferable that electrode matrix uses glass-carbon electrode.Need explanation
, glass-carbon electrode is the abbreviation of glassy carbon electrode, and its advantage is good conductivity, and chemically stable is high, and thermal coefficient of expansion is small, quality
Hard, air-tightness is good, therefore it can be seen that can to greatest extent lift electrode using glass-carbon electrode as electrode matrix
Comprehensive performance.
The embodiment of the present invention also proposed a kind of sensor, and it includes above-mentioned electrode.It should be noted that electrode is used
In in the sensor, in especially for use in electrochemical sensor, itself excellent chemical property can be fully played, makes electrification
Sensor is learned to reach high accuracy, high sensitivity and efficiently test and analyze effect.
The embodiment of the present invention also proposed one kind using the sensor in detection Cu2+In application.It should be noted that
For detecting Cu2+Sensor be electrochemical sensor, in addition, why detecting Cu using above-mentioned sensor2+, be because
It is to utilize Cu2+Sulfydryl can be catalyzed make disulphide this principles of chemistry can set up super sensitivity detection Cu2+Electrification
Sensor is learned, and this electrochemical sensor is simple to operate and friendly to environment, the linear model of sensitivity and non-constant width with superelevation
Enclose, this is detection Cu2+There is provided a kind of new method.
Feature of the invention and performance are described in further detail with reference to embodiments.
Embodiment 1
The present embodiment provides a kind of electrode, and it includes glass-carbon electrode and is arranged at the nanometer composite layer of glassy carbon electrode surface,
Wherein, nanometer composite layer is made up of nitrogen-doped graphene-silver Jenner's nano composite material.
Further, the preparation process of nitrogen-doped graphene-silver Jenner's nano composite material is：First, by the graphite oxide of 5mg
Alkene is distributed in 5mL ultra-pure waters, obtains graphene oxide water solution.Then, added in the graphene oxide water solution for obtaining
The μ L of silver nitrate solution 100 of 0.1mol/L, and carry out 50 DEG C of Ultrasonic Heating 1h.Afterwards, the chlorine gold that mass fraction is 1% is added
The μ L of acid solution 500, followed by, add the stirring of 500mg carbons ammonia to dissolve it, then by mixed liquor immigration autoclave
130 DEG C of reaction 10h.Finally with ultra-pure water centrifuge washing repeatedly, until the pH of supernatant be 7 or so after, the precipitation that will be obtained
It is placed in vacuum drying chamber, and 12h is vacuum dried at 60 DEG C.
The present embodiment additionally provides a kind of preparation method of the electrode for implementing to provide, and its preparation process is as follows：Use respectively
After 1.0 μm, 0.3 μm and 0.05 μm of alumina powder is polished to glass-carbon electrode successively, then carried out with ethanol and distilled water
Supersound washing, is dried up with nitrogen afterwards；Nitrogen-doped graphene in the present embodiment-silver Jenner's nano composite material is configured to 1.0g/L
Solution, then with liquid-transfering gun draw 5 μ L equably drop coating in glassy carbon electrode surface, dry naturally at room temperature, do not make usually
Used time can be preserved under conditions of 4 DEG C.
The present embodiment additionally provides a kind of sensor, and it is in particular electrochemical sensor, its by above-mentioned electrode, Pt
Electrode and 0.1mol/L, pH are 7.4 Tris-HCl solution compositions, wherein, above-mentioned electrode as electrochemical sensor work
Make electrode, Pt electrode as electrochemical sensor counterelectrode, Tris-HCl solution serves as the electrolyte of electrochemical sensor
Layer.
Embodiment 2
The present embodiment provides a kind of electrode, and it includes glass-carbon electrode and is arranged at the nanometer composite layer of glassy carbon electrode surface,
Wherein, nanometer composite layer is made up of nitrogen-doped graphene-silver Jenner's nano composite material.
Further, the preparation process of nitrogen-doped graphene-silver Jenner's nano composite material is：First, by the graphite oxide of 4mg
Alkene is distributed in 5mL ultra-pure waters, obtains graphene oxide water solution.Then, added in the graphene oxide water solution for obtaining
The μ L of silver nitrate solution 100 of 0.08mol/L, and carry out 50 DEG C of Ultrasonic Heating 1h.Afterwards, it is 0.8% to add mass fraction
The μ L of chlorauric acid solution 500, followed by, add the stirring of 490mg carbons ammonia to dissolve it, and mixed liquor then is moved into autoclave
In 130 DEG C reaction 10h.Centrifuge washing with ultra-pure water repeatedly, it is heavy by what is obtained until the pH of supernatant is after 7 or so finally
Shallow lake is placed in vacuum drying chamber, and is vacuum dried 12h at 60 DEG C.
The present embodiment additionally provides a kind of preparation method of the electrode for implementing to provide, and its preparation process is as follows：Use respectively
After 1.0 μm, 0.3 μm and 0.05 μm of alumina powder is polished to glass-carbon electrode successively, then carried out with ethanol and distilled water
Supersound washing, is dried up with nitrogen afterwards；Nitrogen-doped graphene in the present embodiment-silver Jenner's nano composite material is configured to 0.9g/L
Solution, then with liquid-transfering gun draw 5 μ L equably drop coating in glassy carbon electrode surface, dry naturally at room temperature, do not make usually
Used time can be preserved under conditions of 4 DEG C.
Embodiment 3
The present embodiment provides a kind of electrode, and it includes glass-carbon electrode and is arranged at the nanometer composite layer of glassy carbon electrode surface,
Wherein, nanometer composite layer is made up of nitrogen-doped graphene-silver Jenner's nano composite material.
Further, the preparation process of nitrogen-doped graphene-silver Jenner's nano composite material is：First, by the graphite oxide of 6mg
Alkene is distributed in 5mL ultra-pure waters, obtains graphene oxide water solution.Then, added in the graphene oxide water solution for obtaining
The μ L of silver nitrate solution 100 of 0.12mol/L, and carry out 50 DEG C of Ultrasonic Heating 1h.Afterwards, it is 1.2% to add mass fraction
The μ L of chlorauric acid solution 500, followed by, add the stirring of 510mg carbons ammonia to dissolve it, and mixed liquor then is moved into autoclave
In 130 DEG C reaction 10h.Centrifuge washing with ultra-pure water repeatedly, it is heavy by what is obtained until the pH of supernatant is after 7 or so finally
Shallow lake is placed in vacuum drying chamber, and is vacuum dried 12h at 60 DEG C.
The present embodiment additionally provides a kind of preparation method of the electrode for implementing to provide, and its preparation process is as follows：Use respectively
After 1.0 μm, 0.3 μm and 0.05 μm of alumina powder is polished to glass-carbon electrode successively, then carried out with ethanol and distilled water
Supersound washing, is dried up with nitrogen afterwards；Nitrogen-doped graphene in the present embodiment-silver Jenner's nano composite material is configured to 1.1g/L
Solution, then with liquid-transfering gun draw 5 μ L equably drop coating in glassy carbon electrode surface, dry naturally at room temperature, do not make usually
Used time can be preserved under conditions of 4 DEG C.
Test example
In order to the performance to electrode in the embodiment of the present invention carries out test verification, this test example chooses the electrification of embodiment 1
Sensor is learned as the sample of this test example, Cu is applied to2+Detection in carry out experimental analysis test.
Further, test example has carried out Cu for the electrochemical sensor prepared in embodiment 12+Electrochemical Detection.
Specifically, by the Cu of 400 μ L2+Solution and the L-Cys solution mixing 30min that 400 μ L molar concentrations are 15 μM, make L-Cys by Cu2 +And O2Catalysis oxidation is cystamine, the electrochemical sensor 25min for then being prepared in full leaching embodiment 1 thereto, finally using poor
Dividing pulse voltammetry (DPV) carries out Electrochemical Detection analysis.It should be noted that carrying out the electrochemistry work of Electrochemical Detection analysis
Make station model CHI 660E, when being tested using DPV methods, potential range is 0-0.4V, and so test experiments exist
Room temperature is carried out.
Further, electrochemical Characterization is carried out to the electrochemical sensor of embodiment 1 using cyclic voltammetry (CV), is tied
Fruit refer to Fig. 1.That a-d curves are represented respectively in Fig. 1 is bare electrode, NG-AgAu/GCE, submerge in the L-Cys solution after
NG-AgAu/GCE, in L-Cys and Cu2+NG-AgAu/GCE after being submerged in mixed solution, comparison curves a, b, c, d can send out
Existing, there is not redox peaks (curve a), after the modification of NG-AgAu materials is carried out to bare electrode, in 0.01V in bare electrode
One group of Strong oxdiative reduction peak (curve b) is occurred in that with 0.2V or so.But when NG-AgAu/GCE is immersed in 15 μM of L-Cys solution
After 25min, oxidation peak current is obviously reduced, and reduction peak current is substantially without (curve c).And work as NG-AgAu/GCE and be immersed in
15 μM of L-Cys solution and Cu2+In mixed solution after 25min, oxidation peak and reduction peak current have increased again compared to curve c
Plus, but still it is smaller than curve b.Therefore, be may certify that nitrogen-doped graphene-silver gold nano by a curves and b curves of Fig. 1
After composite is as the composite Nano layer of electrode, the electrochemical sensor that the electrode is constituted has excellent electrochemistry
Energy；By comparison curves c and d, it is possible to determine that exactly because Cu2+The sulfydryl that L-Cys can be contained carries out catalysis and makes
Disulphide, so as to Cu could be proved in turn2+The presence of itself, this is also to detect whether there is Cu2+Principle where.
In addition, the optimum experimental condition that this test example has also further explored electrochemical sensor is：L-Cys's is dense
Spend is 15 μM, Cu2+The reaction time for being catalyzed L-Cys is 30min, and electrode Immersion time is 30min, and with this optimum experimental condition
Emphasis determines Cu2+The DPV figures of concentration.Reference picture 2 is as can be seen that with Cu2+The increase of concentration, the oxidation peak current of AgNPs
Constantly increase.In concentration range 1-1 × 10-6In nM, the oxidation peak current and Cu of AgNPs2+Concentration is linear, linear to return
The equation is returned to be：Ipa(μ A)=0.7055+0.015 × c (nM), (R=0.998), detection is limited to 0.3nM (S/N=3).
Further, this test example has also listed conventional detection Cu2+Method, and by its electrochemistry with this test example
Sensor test is compared, and concrete outcome is as shown in table 1.
The results contrast of 1 inspection method of test example electrochemical sensor of table and other inspection methods
As can be seen from Table 1, the Cu for being carried out using the electrochemical sensor of this test example2+Detection limit only has in detection process
0.3nM, shows superpower sensitivity, and the range of linearity is related to 1 × 10-6- 1nM, compared to other existing inspections
Method shows the range of linearity of non-constant width.
In a word, the nanometer composite layer of electrode is made based on nitrogen-doped graphene-silver Jenner's nano composite material so that include this
The electrochemical sensor of electrode shows good chemical property, and the electrochemical sensor is applied into Cu2+Detection
In so that its sensitivity for showing superelevation and the range of linearity very wide.
In sum, the embodiment of the present invention is set by nitrogen-doped graphene-silver gold nano composite wood by electrode matrix
The nanometer composite layer that material is made is so that the chemical property and catalytic performance of this electrode are improved；By simple drop coating side
Method so that preparing the technique of the electrode becomes extremely simple；Therefore, including above-mentioned electrode electrochemical sensor, it is not only grasped
Make simple, environment-friendly, and the sensitivity with superelevation and non-constant width the range of linearity, it is used for Cu2+Detection in, performance
Good chemical property and catalytic performance is gone out.
Embodiments described above is a part of embodiment of the invention, rather than whole embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
1. a kind of electrode, it is characterised in that the electrode includes electrode matrix and is arranged at the nanometer on the electrode matrix surface
Composite bed, the nanometer composite layer is made up of nitrogen-doped graphene-silver Jenner's nano composite material.
2. electrode according to claim 1, it is characterised in that the nitrogen-doped graphene-silver Jenner's nano composite material be by
It is made after silver nitrate solution, graphene oxide solution, chlorauric acid solution and carbonic acid ammonia hybrid reaction.
3. electrode according to claim 2, it is characterised in that the concentration of the silver nitrate solution is 0.08-0.12mol/
L；The mass concentration of the graphene oxide solution is 0.8-1.2g/L；The quality percentage of the gold chloride in the chlorauric acid solution
Than being 0.8%-1.2%.
4. electrode according to claim 3, it is characterised in that silver nitrate, the oxidation stone in the silver nitrate solution
The mass ratio of gold chloride in graphene oxide, the chlorauric acid solution and the carbonic acid ammonia in black alkene solution is 1.6-1.8：
0.8-1.2：4.8-5.2：490-510.
5. the preparation method of a kind of electrode as described in claim 1-4 any one, it is characterised in that it includes following step
Suddenly：
After the electrode matrix is polished, washs and is dried successively, by the nitrogen-doped graphene-silver Jenner's nano composite material
Water-soluble drop-coated on the electrode matrix, and carry out nature and dry.
6. the preparation method of electrode according to claim 5, it is characterised in that the electrode matrix is glass-carbon electrode.
7. the preparation method of electrode according to claim 5, it is characterised in that the nitrogen-doped graphene-silver gold nano is answered
The aqueous solution mass concentration of condensation material is 0.9-1.1g/L.
8. a kind of sensor, it is characterised in that it includes the electrode as described in claim any one of 1-4.
9. sensor according to claim 8, it is characterised in that the sensor is electrochemical sensor.
10. the sensor described in claim 9 is in detection Cu2+In application.
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| CN110441358B (en) * | 2019-07-10 | 2021-08-13 | 云南大学 | Method for detecting iodide ions based on graphene/gold @ silver nanoparticle modified electrode |
| CN115184424A (en) * | 2022-07-08 | 2022-10-14 | 湖南大学 | Method for detecting lead, detection electrode, electrochemical sensor and preparation |
| CN115184424B (en) * | 2022-07-08 | 2024-01-16 | 湖南大学 | Method for detecting lead, detection electrode, electrochemical sensor and preparation method |
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