CN107237008A - Preparation method, electrode and the electrochemical sensor of porous nano-fibre - Google Patents
Preparation method, electrode and the electrochemical sensor of porous nano-fibre Download PDFInfo
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- CN107237008A CN107237008A CN201710404070.7A CN201710404070A CN107237008A CN 107237008 A CN107237008 A CN 107237008A CN 201710404070 A CN201710404070 A CN 201710404070A CN 107237008 A CN107237008 A CN 107237008A
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Classifications
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
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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
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
Abstract
This application discloses a kind of preparation method of porous nano-fibre, electrode and electrochemical sensor, the preparation method of porous nano-fibre includes：(1) deionized water, is added to polyvinylpyrrolidone, uniform, transparent aqueous povidone solution is obtained；(2), by La (NO3)3·6H2O and Co (CH3COO)2·4H2O, which is uniformly mixed and is dissolved in deionized water, obtains inorganic salt solution；(3), aqueous povidone solution and inorganic salt solution are mixed, magnetic agitation 15~20 hours, obtain the colloidal sol shape spinning solution of certain viscosity at room temperature；(4), by spinning solution electrostatic spinning；(5), in 70~90 DEG C of freeze-day with constant temperature 8~10 hours；(6) 500 DEG C, are warming up to 1.5~2 DEG C/min, constant temperature 1.5~2 hours, then heat treatment temperature is risen to 600 DEG C with 0.5 DEG C/min heating rates, calcine 3~5 hours, obtain LaCoO3Porous hollow nano fiber.Inventive sensor is used for L tryptophan Electrochemical Detections, with higher sensitivity and very low detection limit, and the sensor also has good long-time stability.
Description
Technical field
The application is related to a kind of sensor, more particularly to a kind of preparation method of porous nano-fibre, electrode and electrification
Learn sensor.
Background technology
The formula of perovskite-type rare-earth composite oxides is ABO3, wherein A is thulium or alkaline-earth metal member
Element, B is transition metal, and O is oxygen element.Perovskite-type rare-earth composite oxides are a kind of important depollution of environment catalysis
Agent, it all has good catalytic action to carbon monoxide, methane, ethane and nitrogen oxides, for being catalyzed burning, vehicle exhaust
Purification and flue gas desulfurization etc..
Tryptophan, as one of common 20 kinds of amino acid of constitutive protein matter, is mammal essential amino acid and raw sugar
Amino acid.Due to tryptophan, amount is fewer in fruits and vegetables, can not be synthesized in human body, so being often added to food
In medicine, but excessive edible tryptophan can cause brain metabolism poisoning, may result in and suffer from psychotic disorder, therefore build
A kind of accurate, quick, simple method is used to detect that the tryptophan in food is very important.
The content of the invention
It is an object of the invention to provide a kind of preparation method of porous nano-fibre, electrode and electrochemical sensor, with
Overcome deficiency of the prior art.
To achieve the above object, the present invention provides following technical scheme：
The embodiment of the present application discloses a kind of preparation method of porous nano-fibre, including step：
(1) deionized water, is added to polyvinylpyrrolidone, uniform, transparent aqueous povidone solution is obtained；
(2), by La (NO3)3·6H2O and Co (CH3COO)2·4H2O, which is uniformly mixed and is dissolved in deionized water, obtains inorganic
Saline solution；
(3), aqueous povidone solution and inorganic salt solution are mixed, magnetic agitation 15~20 is small at room temperature
When, obtain the colloidal sol shape spinning solution of certain viscosity；
(4), by spinning solution electrostatic spinning；
(5), in 70~90 DEG C of freeze-day with constant temperature 8~10 hours；
(6) 500 DEG C, are warming up to 1.5~2 DEG C/min, constant temperature 1.5~2 hours, then will with 0.5 DEG C/min heating rates
Heat treatment temperature rises to 600 DEG C, calcines 3~5 hours, obtains LaCoO3Porous hollow nano fiber.
It is preferred that, in the preparation method of above-mentioned porous nano-fibre, in the step (3), polyvinylpyrrolidone
Weight is in 30~40%, La (NO3)3·6H2O and Co (CH3COO)2·4H2O weight ratio is 8~12%.
It is preferred that, in the preparation method of above-mentioned porous nano-fibre, in the step (4), electrospinning conditions are full
Foot：10~15kV of voltage, syringe needle to receiver distance is 10~15cm.
Disclosed herein as well is a kind of electrode, it is characterised in that including electrode matrix and is coated on electrode matrix surface
Described porous nano-fibre.
It is preferred that, in above-mentioned electrode, the electrode matrix is carbon paste electrode.
Disclosed herein as well is a kind of electrochemical sensor, it is characterised in that is used as working electrode using described electrode.
Compared with prior art, the advantage of the invention is that：Inventive sensor is used for L-Trp Electrochemical Detection,
LaCoO3The electrode pair L-Trp of porous hollow nano fiber modification has excellent electrocatalysis, by the sensor of its making
With higher sensitivity and very low detection limit, sensor to L-Trp linear response range at 0.03~6 μM, minimum inspection
Rising limit is at 0.01 μM.The sensor also has good long-time stability.
Embodiment
The present invention is described further by the following example：According to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described by embodiment are only used
In the explanation present invention, without should be also without limitation on the present invention described in detail in claims.
In one embodiment, the preparation method of porous nano-fibre, including：
(1) deionized water, is added to polyvinylpyrrolidone, uniform, transparent aqueous povidone solution is obtained；
(2), by La (NO3)3·6H2O and Co (CH3COO)2·4H2O, which is uniformly mixed and is dissolved in deionized water, obtains inorganic
Saline solution；
(3), aqueous povidone solution and inorganic salt solution are mixed, at room temperature magnetic agitation 20 hours,
The colloidal sol shape spinning solution of certain viscosity is obtained, wherein polyvinylpyrrolidone weight is in 30~40%, La (NO3)3·6H2O and
Co(CH3COO)2·4H2O weight ratio is 8~12%；
(4), by spinning solution electrostatic spinning, 10~15kV of applied voltage, syringe needle to receiver distance is 10~15cm；
(5), in 70~90 DEG C of freeze-day with constant temperature 8~10 hours；
(6) 500 DEG C, are warming up to 1.5~2 DEG C/min, constant temperature 1.5~2 hours, then will with 0.5 DEG C/min heating rates
Heat treatment temperature rises to 600 DEG C, calcines 3~5 hours, obtains LaCoO3Porous hollow nano fiber, it has smooth surface,
Configuration of surface is homogeneous, 100~150nm of external diameter, and thickness of pipe wall is 30~50nm, and length is more than 80 μm.
(7), by obtained LaCoO3Porous hollow nano fiber is dispersed in water, and coating liquid is made, then by coating liquid
Electrode matrix surface is coated in, LaCoO is obtained3The electrode of porous hollow nano fiber modification, electrode matrix is carbon paste electrode；
(8), with LaCoO3The electrode of porous hollow nano fiber modification makes electrochemical sensor as working electrode.
The sensor is used for L-Trp Electrochemical Detection, LaCoO3The electrode pair L- colors of porous hollow nano fiber modification
Propylhomoserin has excellent electrocatalysis, has higher sensitivity and very low detection limit, sensor by the sensor of its making
To L-Trp linear response range at 0.03~6 μM, minimum detectability is at 0.01 μM.The sensor also has well long-term
Stability.
Finally, in addition it is also necessary to explanation, term " comprising ", "comprising" or its any other variant are intended to non-exclusive
Property include so that process, method, article or equipment including a series of key elements not only include those key elements, and
Also include other key elements for being not expressly set out, or also include for this process, method, article or equipment inherently
Key element.
Claims (6)
1. a kind of preparation method of porous nano-fibre, it is characterised in that including step：
(1) deionized water, is added to polyvinylpyrrolidone, uniform, transparent aqueous povidone solution is obtained；
(2), by La (NO3)3·6H2O and Co (CH3COO)2·4H2O, which is uniformly mixed and is dissolved in deionized water, obtains inorganic salt solution
Solution；
(3), aqueous povidone solution and inorganic salt solution are mixed, at room temperature magnetic agitation 15~20 hours,
Obtain the colloidal sol shape spinning solution of certain viscosity；
(4), by spinning solution electrostatic spinning；
(5), in 70~90 DEG C of freeze-day with constant temperature 8~10 hours；
(6) 500 DEG C, are warming up to 1.5~2 DEG C/min, constant temperature 1.5~2 hours, then will be at heat with 0.5 DEG C/min heating rates
Reason temperature rises to 600 DEG C, calcines 3~5 hours, obtains LaCoO3Porous hollow nano fiber.
2. the preparation method of porous nano-fibre according to claim 1, it is characterised in that：In the step (3), poly- second
Alkene pyrrolidone weight is in 30~40%, La (NO3)3·6H2O and Co (CH3COO)2·4H2O weight ratio is 8~12%.
3. the preparation method of porous nano-fibre according to claim 1, it is characterised in that：In the step (4), electrostatic
Spinning condition is met：10~15kV of voltage, syringe needle to receiver distance is 10~15cm.
4. a kind of electrode, it is characterised in that appoint including electrode matrix and the claims 1 to 3 for being coated on electrode matrix surface
Porous nano-fibre described in one.
5. electrode according to claim 4, it is characterised in that：The electrode matrix is carbon paste electrode.
6. a kind of electrochemical sensor, it is characterised in that working electrode is used as using the electrode described in claim 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710404070.7A CN107237008A (en) | 2017-06-01 | 2017-06-01 | Preparation method, electrode and the electrochemical sensor of porous nano-fibre |
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| CN201710404070.7A CN107237008A (en) | 2017-06-01 | 2017-06-01 | Preparation method, electrode and the electrochemical sensor of porous nano-fibre |
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| CN201710404070.7A Pending CN107237008A (en) | 2017-06-01 | 2017-06-01 | Preparation method, electrode and the electrochemical sensor of porous nano-fibre |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109913971A (en) * | 2017-12-12 | 2019-06-21 | 中国科学院大连化学物理研究所 | A kind of porous composite nano fiber and its preparation method and application |
| CN112110497A (en) * | 2020-09-28 | 2020-12-22 | 中国科学技术大学 | Lanthanide metal-doped lanthanum cobaltate type nanotube material, preparation method thereof and method for producing hydrogen by electrolyzing water |
Citations (7)
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| CN101787574A (en) * | 2010-03-04 | 2010-07-28 | 长春理工大学 | Method for preparing lanthanum hydroxide porous hollow nano-fiber and chain-like nano-fiber |
| CN102021677A (en) * | 2010-10-13 | 2011-04-20 | 清华大学 | Preparation method for carbon nanofiber containing transition metal and nitrogen element and application of carbon nanofiber in fuel-cell catalysts |
| CN103789876A (en) * | 2014-01-24 | 2014-05-14 | 山西师范大学 | Synthetic method of strip porous lanthanum ferrite nano fibers |
| CN104752069A (en) * | 2013-12-31 | 2015-07-01 | 西北大学 | Preparation method of metallic oxide or metallic oxide composite material |
| CN104775185A (en) * | 2015-04-14 | 2015-07-15 | 济南大学 | Cobaltosic oxide bead-chain-shaped fiber and preparation method thereof |
| CN106192081A (en) * | 2016-06-30 | 2016-12-07 | 天津工业大学 | A kind of preparation method of Graphene skeletal porous nanofiber |
| CN106784745A (en) * | 2017-03-02 | 2017-05-31 | 西京学院 | The sodium-ion battery method for manufacturing electric spinning of cobaltosic oxide carbon nano-fiber |
-
2017
- 2017-06-01 CN CN201710404070.7A patent/CN107237008A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101787574A (en) * | 2010-03-04 | 2010-07-28 | 长春理工大学 | Method for preparing lanthanum hydroxide porous hollow nano-fiber and chain-like nano-fiber |
| CN102021677A (en) * | 2010-10-13 | 2011-04-20 | 清华大学 | Preparation method for carbon nanofiber containing transition metal and nitrogen element and application of carbon nanofiber in fuel-cell catalysts |
| CN104752069A (en) * | 2013-12-31 | 2015-07-01 | 西北大学 | Preparation method of metallic oxide or metallic oxide composite material |
| CN103789876A (en) * | 2014-01-24 | 2014-05-14 | 山西师范大学 | Synthetic method of strip porous lanthanum ferrite nano fibers |
| CN104775185A (en) * | 2015-04-14 | 2015-07-15 | 济南大学 | Cobaltosic oxide bead-chain-shaped fiber and preparation method thereof |
| CN106192081A (en) * | 2016-06-30 | 2016-12-07 | 天津工业大学 | A kind of preparation method of Graphene skeletal porous nanofiber |
| CN106784745A (en) * | 2017-03-02 | 2017-05-31 | 西京学院 | The sodium-ion battery method for manufacturing electric spinning of cobaltosic oxide carbon nano-fiber |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109913971A (en) * | 2017-12-12 | 2019-06-21 | 中国科学院大连化学物理研究所 | A kind of porous composite nano fiber and its preparation method and application |
| CN112110497A (en) * | 2020-09-28 | 2020-12-22 | 中国科学技术大学 | Lanthanide metal-doped lanthanum cobaltate type nanotube material, preparation method thereof and method for producing hydrogen by electrolyzing water |
| CN112110497B (en) * | 2020-09-28 | 2022-04-19 | 中国科学技术大学 | Lanthanide metal-doped lanthanum cobaltate type nanotube material, preparation method thereof and method for producing hydrogen by electrolyzing water |
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