CN102661981A - Preparation method of NOx detection electrochemical sensor - Google Patents
Preparation method of NOx detection electrochemical sensor Download PDFInfo
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- CN102661981A CN102661981A CN2012100916377A CN201210091637A CN102661981A CN 102661981 A CN102661981 A CN 102661981A CN 2012100916377 A CN2012100916377 A CN 2012100916377A CN 201210091637 A CN201210091637 A CN 201210091637A CN 102661981 A CN102661981 A CN 102661981A
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Abstract
The invention relates to a preparation method of an NOx detection electrochemical sensor. The preparation method is characterized in that a platinum electrode washed by secondary deionized water is pretreated by H2SO4 at a sweep potential of -0.2 to +1.45V 10 times and then is washed by secondary deionized water and the clean platinum electrode is connected to single-walled carbon nanotube (SWCNT)-polypyrrole (PPy); and the preparation method concretely comprises the following steps of forming a PPy film on a platinum electrode, carrying out oxidation of 0.4mol/L of a pyrrole solution in 0.1mol/L of a KCl solution in an argon atmosphere, repeating oxidation 10 times, dropwisely adding 25 microlitres of a SWCNT solution on the PPy-modified platinum electrode surface, carrying out ethanol evaporation to obtain a SWCNT-PPy nanocomplex, and depositing Cu nanoparticles (CuNP) on a SWCNT-PPy-Pt electrode by an electrochemical deposition method based on 0.1mol/L of KCL as a support electrode to obtain a CuNP-SWCNT-PPy-Pt-based electrode sensor. The CuNP-SWCNT-PPy-Pt-based electrode sensor has good repeatability and maintains good stability in a month.
Description
Technical field:
The present invention relates to a kind of preparation method of electrochemical sensor, relate in particular to a kind of preparation method of the NOx of detection electrochemical sensor.
Background technology:
Nitrogen monoxide is being brought into play important effect at blood vessel biology and pathobiology.NO is a kind of neuron signaling molecule in central authorities and nervus peripheralis system, and it can be synthetic by mammalian cell.In addition, NO can also play the part of physiological " bearer " and cytotoxic " procurator ".NO is very unstable, and the half life period has only 2～30s to react generation NOx (NO and NO with oxygen molecule rapidly
2).So, have high sensitivity and accuracy and detect NO
xMethod be essential.
A lot of methods are used to detect NO
x, such as electron paramagnetic resonance, spectrophotometry de termination and chemoluminescence method.In all methods, electrochemical method is simple, light owing to having, and advantage cheap and express-analysis is proved to be a kind of very strong method.Method with resistance, voltage and current detects NO
xSome reports have been arranged.Recently, ZnO-In
2O
3Film is used for detecting NO widely
xGas.But corresponding sensor does not but have high sensitivity and its use to need very high temperature (200-500 ℃).
CNT (CNTs) has been used in the sensor widely, because they have good chemical stability, outstanding electronics and mechanical property.These special nature make CNT can be good at the support as inorganic nano material, such as the copper nano particles that can be used as electrochemical sensor (CuNP).CNT has high conductivity and big surface area, therefore can promote the performance of copper nano particles.Directly be prepared into copper nano particles that a very big advantage is arranged on the CNT is exactly the performance that has kept nanocrystal and nanotube self.
Therefore but at electrode surface combining nano particle and nanotube is a very big difficult problem, need find at present a kind of copper nano particles (CuNP) to be incorporated on the platinum electrode (CuNP-SWCNT-PPy-Pt) that SWCNT-PPy modifies, and be used for detecting NO
xElectrochemical sensor.
Summary of the invention:
The present invention is directed to the deficiency of prior art, a kind of preparation method of the NOx of detection electrochemical sensor is provided.
A kind of preparation method who detects the NOx electrochemical sensor, its making step is following:
(1) pre-service: before experiment, with diameter be the platinum electrode of 0.5mm earlier with the aluminium powder polishing, wash twice with secondary deionized water then; The platinum electrode of wash clean is with the H of 1mol/L
2SO
4Be-0.2 at the scanning electromotive force～+ scope of 1.45V in pre-service 10 times, wash with secondary deionized water then; Before the electrochemical polymerization reaction of at every turn carrying out the pyrroles, all to carry out same pre-service;
(2) preparation method: on platinum electrode, connect SWCN-polypyrrole; At first; Pyrrole polymerization forms the film of polypyrrole on platinum electrode: the setting potential range is 0～0.9V (is reference with the Ag/AgCl electrode); Under argon atmosphere, pyrroles's solution of oxidation 0.4mol/L in the KCl of 0.1mol/L solution, circulation is carried out 10 times; Then, the solution of 25 μ L SWCNs (SWCNT) is dripped to the platinum electrode surface of polypyrrole modifying, form the SWCNT-PPy nano-complex after the ethanol evaporation; At last with the KCl of 0.1mol/L as support electrode, set potential range and be-0.4～+ 0.9V (is reference with the Ag/AgCl electrode), with the CuCl of 0.1mol/L
2As copper raw material, utilize the method for electrochemical deposition that copper nano-particle (CuNP) is deposited on the SWCNT-PPy-Pt electrode, form based on the CuNP-SWCNT-PPy-Pt electrode sensor.
The solution of said SWCN (SWCNT) is: 2mg SWCNT+1ml 0.5wt%nafion-ethanolic solution.
Characterizing with scanning electron microscope and the analysis of X-ray energy spectrum of the present invention's design based on the CuNP-SWCNT-PPy-Pt electrode sensor; With cyclic voltammetry the electrochemical properties of the electrode that designed is studied; Experiment shows: found the reversible redox peak of copper nano particles (CuNP), the electrode pair NO of design at-0.15V and-0.3V
xThe electro-catalysis ability be four times of CuNP-PPy-Pt electrode, testing result shows that clearly SWCN polypyrrole nano-complex (SWCNT-PPy) can promote the electron transport between copper nano particles and the platinum electrode.In addition, sensor sheet has revealed extraordinary repeatable ability and in one month time, has all kept good stability.
Description of drawings:
Fig. 1 is preparation of the present invention, reaction synoptic diagram
Embodiment:
In order to deepen, the present invention is made further detailed description below in conjunction with implementing to understanding of the present invention.
A kind of preparation method who detects the NOx electrochemical sensor, its step is following:
(1) before experiment, with diameter be the platinum electrode of 0.5mm earlier with the aluminium powder polishing, wash twice with secondary deionized water then; The platinum electrode of wash clean is with the H of 1mol/L
2SO
4Be-0.2 at the scanning electromotive force～+ scope of 1.45V in pre-service 10 times, wash with secondary deionized water then; Before the electrochemical polymerization reaction of at every turn carrying out the pyrroles, all to carry out same pre-service.
(2) on platinum electrode, connect SWCN-polypyrrole; At first; Pyrrole polymerization forms the film of polypyrrole on platinum electrode: the setting potential range is 0～0.9V (is reference with the Ag/AgCl electrode); Under argon atmosphere, pyrroles's solution of oxidation 0.4mol/L in the KCl of 0.1mol/L solution, circulation is carried out 10 times; Then, the solution (2mg SWCNT+1ml 0.5wt%nafion-ethanolic solution) of 25 μ L SWCNs (SWCNT) is dripped to the platinum electrode surface of polypyrrole modifying, form the SWCNT-PPy nano-complex after the ethanol evaporation; At last with the KCl of 0.1mol/L as support electrode, set potential range and be-0.4～+ 0.9V (is reference with the Ag/AgCl electrode), with the CuCl of 0.1mol/L
2As copper raw material, utilize the method for electrochemical deposition that copper nano-particle (CuNP) is deposited on the SWCNT-PPy-Pt electrode, form based on the CuNP-SWCNT-PPy-Pt electrode sensor.
Claims (2)
1. preparation method who detects the NOx electrochemical sensor, it is characterized in that: making step is following:
(1) pre-service: before experiment, with diameter be the platinum electrode of 0.5mm earlier with the aluminium powder polishing, wash twice with secondary deionized water then; The platinum electrode of wash clean is with the H of 1mol/L
2SO
4Be-0.2 at the scanning electromotive force～+ scope of 1.45V in pre-service 10 times, wash with secondary deionized water then; Before the electrochemical polymerization reaction of at every turn carrying out the pyrroles, all to carry out same pre-service;
(2) preparation method: on platinum electrode, connect SWCN-polypyrrole; At first, the film of pyrrole polymerization formation polypyrrole on platinum electrode: the setting potential range is 0～0.9V, under argon atmosphere; Pyrroles's solution of oxidation 0.4mol/L in the KCl of 0.1mol/L solution, circulation is carried out 10 times; Then, the solution of 25 μ L SWCN-SWCNT is dripped to the platinum electrode surface of polypyrrole modifying, form the SWCNT-PPy nano-complex after the ethanol evaporation; At last with the KCl of 0.1mol/L as support electrode, set potential range and be-0.4～+ 0.9V, with the CuCl of 0.1mol/L
2As copper raw material, utilize the method for electrochemical deposition that copper nano-particle-CuNP is deposited on the SWCNT-PPy-Pt electrode, form based on the CuNP-SWCNT-PPy-Pt electrode sensor.
2. a kind of preparation method who detects the NOx electrochemical sensor according to claim 1, it is characterized in that: the solution of SWCN-SWCNT is: 2mg SWCNT+1ml 0.5wt%nafion-ethanolic solution.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014194484A1 (en) * | 2013-06-05 | 2014-12-11 | 中国科学院微电子研究所 | Manufacturing method of no2 gas sensor for detection at room temperature |
| CN107817287A (en) * | 2017-10-30 | 2018-03-20 | 上海应用技术大学 | A kind of sensor of detection nitrogen oxides based on nano graphene oxide and preparation method thereof |
| CN110153403A (en) * | 2018-02-13 | 2019-08-23 | 中国石油化工股份有限公司 | Copper@polypyrrole nano line and preparation method thereof and pressure drag material and its application |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102081067A (en) * | 2011-02-16 | 2011-06-01 | 西安交通大学 | Carbon nanotube (CNT) film based ionization nitrogen dioxide sensor and method for measuring concentration by adopting same |
| CN102203593A (en) * | 2008-09-29 | 2011-09-28 | 法国原子能及替代能源委员会 | Chemical sensors containing carbon nanotubes, method for making same, and uses thereof |
-
2012
- 2012-03-31 CN CN2012100916377A patent/CN102661981A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102203593A (en) * | 2008-09-29 | 2011-09-28 | 法国原子能及替代能源委员会 | Chemical sensors containing carbon nanotubes, method for making same, and uses thereof |
| CN102081067A (en) * | 2011-02-16 | 2011-06-01 | 西安交通大学 | Carbon nanotube (CNT) film based ionization nitrogen dioxide sensor and method for measuring concentration by adopting same |
Non-Patent Citations (1)
| Title |
|---|
| SUBASH PRAKASH等: ""Copper nanoparticles entrapped in SWCNT-PPy nanocomposite on Pt electrode as NOx electrochemical sensor"", 《TALANTA》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014194484A1 (en) * | 2013-06-05 | 2014-12-11 | 中国科学院微电子研究所 | Manufacturing method of no2 gas sensor for detection at room temperature |
| US9562884B2 (en) | 2013-06-05 | 2017-02-07 | Institute of Microelectronics, Chinese Academy of Sciences | Method for manufacturing NO2 gas sensor for detection at room temperature |
| CN107817287A (en) * | 2017-10-30 | 2018-03-20 | 上海应用技术大学 | A kind of sensor of detection nitrogen oxides based on nano graphene oxide and preparation method thereof |
| CN110153403A (en) * | 2018-02-13 | 2019-08-23 | 中国石油化工股份有限公司 | Copper@polypyrrole nano line and preparation method thereof and pressure drag material and its application |
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Application publication date: 20120912 |