CN107917939A - Electromagnetism chemical sensor based on conducting polymer and preparation method thereof - Google Patents
Electromagnetism chemical sensor based on conducting polymer and preparation method thereof Download PDFInfo
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- CN107917939A CN107917939A CN201711206997.6A CN201711206997A CN107917939A CN 107917939 A CN107917939 A CN 107917939A CN 201711206997 A CN201711206997 A CN 201711206997A CN 107917939 A CN107917939 A CN 107917939A
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/08—Heat treatment
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/20—Metallic material, boron or silicon on organic substrates
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
Abstract
The present invention provides a kind of electromagnetism chemical sensor based on conducting polymer and preparation method thereof, including step：Oxidant containing ferric ion or over cure acid group is mixed with cationic polyelectrolyte, obtains oxidant/high molecular polymer mixed liquor；Oxidant/high molecular polymer mixed liquor is prepared as oxidant/high molecular polymer loop construction；Oxidant/high molecular polymer loop construction is heat-treated, obtains oxidant/high molecular polymer loop construction with self-supporting effect；Above-mentioned oxidant/high molecular polymer coil is placed in monomer atmosphere and is polymerize, obtains conducting polymer/high molecular polymer loop construction；Conducting polymer/high molecular polymer loop construction both ends are prepared into electrode, so as to obtain a kind of electromagnetism chemical sensor based on conducting polymer.The present invention realizes the fine dispersion of conducting polymer in the composite, so as to ensure that this kind of composite material can be as the sensing unit of electromagnetic sensor.
Description
Technical field
The present invention relates to sensitive material and sensor field, more particularly to a kind of electromagnetism chemistry based on conducting polymer
Sensor and preparation method thereof.
Background technology
Conducting polymer refers to a kind of functional polymer of conductive energy.Adulterated by the methods of chemistry and electrochemistry
The electric conductivity of the polymer significantly improves afterwards, at the same have monovalence to anion or to cation.This high polymer have with
Electricity, the magnetics of the metal performance similar with optics, while the mechanical performance and machinability of traditional high polymer are remained again
Energy.Conductive polymer molecules room-temperature conductivity can change in the range of insulator-semiconductor-metallic state, therefore it is in skill
A variety of attractive prospects are presented in art.
Due to characteristics such as high conductivity, thermal conductivities, traditional copper product preferred material as electromagnetic device always, still
The self-defect of copper product is such as：Carrier skin effect, environmental pollution and rare etc. so that people begin look for common copper product
Substitute.In recent years, the electromagnetic performance of high conductivity polymer gets more and more people's extensive concerning.Due to being carried in conducting polymer
Flow the diversity of son so that this kind of material embodies higher Hall effect coefficient, while the processability that conducting polymer is good
Energy and biocompatible cause it to have tempting development prospect on flexible organic electromagnetic device.In addition, conducting polymer is not
It can only adulterate, but also can go to adulterate, and adulterate/go the process completely reversibility of doping, this to be based on conducting polymer
The electromagnetic device of thing can embody the response characteristic to environmental change, so as to develop the sensing based on its electromagnetic device
Device, is realized to extraneous environmental change such as：High selection, high sensitivity and the reproducible detection of gas, temperature, acid-base property etc..
The content of the invention
The object of the present invention is to provide a kind of simple electromagnetism controllable, of low cost based on conducting polymer of preparation process
Chemical sensor and preparation method thereof.
For achieving the above object, technical solution of the present invention is as follows：
A kind of preparation method of the electromagnetism chemical sensor based on conducting polymer, includes the following steps：
(1) oxidant containing ferric ion or over cure acid group is mixed with cationic polyelectrolyte, obtains uniform oxygen
Agent/high molecular polymer mixed liquor；
(2) oxidant/high molecular polymer mixed liquor is prepared as oxidant/high molecular polymer loop construction；
(3) oxidant/high molecular polymer loop construction is heat-treated, obtains the oxidation with self-supporting effect
Agent/high molecular polymer loop construction；
(4) above-mentioned oxidant/high molecular polymer coil is placed in monomer atmosphere and polymerize, obtain conducting polymer
Thing/high molecular polymer loop construction；
(5) conducting polymer/high molecular polymer loop construction both ends are prepared into electrode, so as to obtain a kind of based on conduction
The electromagnetism chemical sensor of polymer.
It is preferred that self-supporting effect refers to be not required extra substrate and frame to support, in its natural state can
The not changed feature of holding structure shape.
It is preferred that the oxidant is ferric trichloride, toluenesulfonic acid iron, ammonium persulfate one kind therein.
It is preferred that the cationic polyelectrolyte is polystyrolsulfon acid, hydroxypropyl methyl cellulose, polydiene
Diallyidimethylammonium chloride, polyacrylic acid aqueous solution, polyvinyl pyridine butyl quaternary ammonium one kind therein.
It is preferred that the method that loop construction is prepared in step (2) is 3D printing method.
It is preferred that being heat-treated as loop construction to be placed in 195-210 DEG C of water vapor atmosphere in step (3)
In, processing time is 5~10 minutes.
It is preferred that the monomer in step (4) is thiophene, 3,4-rthylene dioxythiophene, aniline, the conjugation of pyrroles are gathered
Close one kind in monomer.
It is preferred that electrode prepared by step (5) is gold, silver, the Copper thin film prepared using vacuum deposition method.
For achieving the above object, the present invention also provides a kind of above-mentioned preparation method obtain based on conducting polymer
Electromagnetism chemical sensor.
The present invention is different from the preparation method of existing conducting polymer electromagnetism chemical sensor, and wherein electromagnetic coil material is
The composite material of conducting polymer and polyelectrolyte, is obtained by way of 3D printing, heat treatment and chemical vapor deposition
Pickup wire coil structures with self-supporting characteristic, regulate and control the size of electric current in coil by the stimulation of external environment change,
Since the change of electric current ultimately results in the change of coil surrounding magnetic field, the detection to extraneous physics, chemical change amount is realized；, should
Sensor construction has good self-supporting characteristic and pliability, can as the sensing unit of flexible electrical Magnetochemical sensor,
And realize integrated and array.
The beneficial outcomes of the present invention are as follows：
(1) electromagnetic sensor coil structural material of the invention is using conducting polymer and highly viscous polyelectrolyte
The mode of Material cladding, enhances the machinability of material, the mode of 3D printing can be utilized arbitrarily to adjust loop construction and circle
Number, loop construction can be strong from renaturation.
(2) present invention realizes the fine dispersion of conducting polymer in the composite by way of heat treatment, so that
It can ensure that composite material still has high conductivity and high Hall effect coefficient, so as to ensure that this kind of composite material can conduct
The sensing unit of electromagnetic sensor
(3) preparation process of the present invention, can be with the preparation work of existing polymer electronics compared to other preparation process
Skill is well compatible, has the broad prospect of application for preparing flexible wearable electromagnetic device.
Embodiment
Illustrate embodiments of the present invention below by way of specific instantiation, those skilled in the art can be by this specification
Disclosed content understands other advantages and effect of the present invention easily.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also be based on different viewpoints with application, without departing from
Various modifications or alterations are carried out under the spirit of the present invention.
Embodiment 1：
Step 1：
Toluenesulfonic acid iron 15mg, diallyl dimethyl ammoniumchloride 10mg are taken, adds 80mL dimethyl sulphoxide solutions
In, using magnetic force heating stirring 30 minutes, obtain toluenesulfonic acid iron/diallyl dimethyl ammoniumchloride solution.
Step 2：
Take 20mL toluenesulfonic acids iron/diallyl dimethyl ammoniumchloride solution and add the syringe needle cavity of 3D printer
In, by default coil pattern printing toluenesulfonic acid iron/diallyl dimethyl ammoniumchloride loop construction, printing speed is
1mm/min。
Step 3：
By toluenesulfonic acid iron/diallyl dimethyl ammoniumchloride coil be placed in 195 DEG C of steam-laden baking ovens into
Row heat treatment, water vapour vapour pressure are 0.5MPa, and processing time is 5 minutes.
Step 4：
Toluenesulfonic acid iron/diallyl dimethyl ammoniumchloride coil is placed in thiophene monomer atmosphere, thiophene monomer
It polymerize, polymerization temperature is 30 DEG C, obtains polythiophene/diallyl dimethyl ammoniumchloride loop construction.
Step 5：Polythiophene/diallyl dimethyl ammoniumchloride coil is placed in vacuum evaporation equipment, in winding head
Enclose and gold electrode is prepared using vacuum deposition method, electrode is the film of thickness 200nm.Final obtain is based on polythiophene/polydiene
The electromagnetism chemical sensor of diallyidimethylammonium chloride coil.
Embodiment 2：
Step 1：
Toluenesulfonic acid iron 15mg, diallyl dimethyl ammoniumchloride 10mg are taken, adds 80mL dimethyl sulphoxide solutions
In, using magnetic force heating stirring 30 minutes, obtain toluenesulfonic acid iron/diallyl dimethyl ammoniumchloride solution.
Step 2：
Take 20mL toluenesulfonic acids iron/diallyl dimethyl ammoniumchloride solution and add the syringe needle cavity of 3D printer
In, by default coil pattern printing toluenesulfonic acid iron/diallyl dimethyl ammoniumchloride loop construction, printing speed is
1mm/min。
Step 3：
By toluenesulfonic acid iron/diallyl dimethyl ammoniumchloride coil be placed in 210 DEG C of steam-laden baking ovens into
Row heat treatment, water vapour vapour pressure are 0.5MPa, and processing time is 10 minutes.
Step 4：
Toluenesulfonic acid iron/diallyl dimethyl ammoniumchloride coil is placed in 3,4- ethene dioxythiophene monomer atmosphere
In, 3,4-rthylene dioxythiophene monomer polymerize, and polymerization temperature is 50 DEG C, obtains poly- 3,4-rthylene dioxythiophene/polydiene
Diallyidimethylammonium chloride loop construction.
Step 5：Poly- 3,4- ethene dioxythiophenes/diallyl dimethyl ammoniumchloride coil is placed in vacuum evaporation equipment
In, silver electrode is prepared using vacuum deposition method in coil head circumference, electrode is the film of thickness 200nm.It is final to obtain based on poly-
The electromagnetism chemical sensor of 3,4- ethene dioxythiophenes/diallyl dimethyl ammoniumchloride coil.
Embodiment 3：
Step 1：
Take ferric trichloride 15mg, hydroxypropyl methyl cellulose 15mg, add in 70mL dimethylformamides, using magnetic force plus
Thermal agitation 30 minutes, obtains toluenesulfonic acid iron/polystyrolsulfon acid solution.
Step 2：
Take 20mL ferric trichlorides/Gonak and add in the syringe needle cavity of 3D printer, by default
Coil pattern prints ferric trichloride/hydroxypropyl methyl cellulose loop construction, and printing speed is 1mm/min.
Step 3：
Ferric trichloride/hydroxypropyl methyl cellulose coil is placed in 200 DEG C of steam-laden baking ovens and is heat-treated, water
Steam vapour pressure is 0.7MPa, and processing time is 6 minutes.
Step 4：
Ferric trichloride/hydroxypropyl methyl cellulose coil is placed in 3,4-rthylene dioxythiophene monomer atmosphere, 3,4- second
Alkene dioxythiophene monomers polymerize, and polymerization temperature is 50 DEG C, obtains poly- 3,4-rthylene dioxythiophene/hydroxypropyl methyl cellulose
Loop construction.
Step 5：Poly- 3,4-rthylene dioxythiophene/hydroxypropyl methyl cellulose coil is placed in vacuum evaporation equipment,
Coil head circumference prepares copper electrode using vacuum deposition method, and electrode is the film of thickness 200nm.Final obtain is based on poly- 3,4- second
The electromagnetism chemical sensor of alkene dioxy thiophene/hydroxypropyl methyl cellulose coil.
Embodiment 4：
Step 1：
Toluenesulfonic acid iron 15mg, polyacrylic acid aqueous solution 15mg are taken, is added in 70mL dimethylformamides, using magnetic force
Heating stirring 30 minutes, obtains toluenesulfonic acid iron/polyacrylic acid solution.
Step 2：
Take 20mL toluenesulfonic acids iron/polyacrylic acid solution and add in the syringe needle cavity of 3D printer, by default coil
Pattern printing toluenesulfonic acid iron/polyacrylic acid loop construction, printing speed is 1mm/min.
Step 3：
Toluenesulfonic acid iron/polyacrylic acid coil is placed in 205 DEG C of steam-laden baking ovens and is heat-treated, water vapour
Vapour pressure is 0.7MPa, and processing time is 7 minutes.
Step 4：
Toluenesulfonic acid iron/polyacrylic acid coil is placed in thiophene monomer atmosphere, thiophene monomer polymerize, polymerization temperature
Spend for 50 DEG C, obtain polythiophene/polyacrylic acid loop construction.
Step 5：Polythiophene/polyacrylic acid coil is placed in vacuum evaporation equipment, vacuum evaporation is used in coil head circumference
Method prepares gold electrode, and electrode is the film of thickness 200nm.Final obtain is based on poly- 3,4- ethene dioxythiophenes/polyacrylic acid
The electromagnetism chemical sensor of coil.
Embodiment 5：
Step 1：
Ammonium persulfate 20mg, polyvinyl pyridine butyl quaternary ammonium 20mg are taken, adds in 100mL n-butanols, is heated using magnetic force
Stirring 30 minutes, obtains ammonium persulfate/polyvinyl pyridine butyl quaternary ammonium solution.
Step 2：
Take 20mL ammonium persulfates/polyvinyl pyridine butyl quaternary ammonium solution and add in the syringe needle cavity of 3D printer, by pre-
If coil pattern prints ammonium persulfate/polystyrolsulfon acid loop construction, printing speed is 1mm/min.
Step 3：
Ammonium persulfate/polyvinyl pyridine butyl quaternary ammonium coil is placed in 200 DEG C of steam-laden baking ovens and is heat-treated,
Water vapour vapour pressure is 0.65MPa, and processing time is 8 minutes.
Step 4：
Ammonium persulfate/polyvinyl pyridine butyl quaternary ammonium coil is placed in aniline monomer atmosphere, aniline monomer polymerize,
Polymerization temperature is 60 DEG C, obtains polyaniline/polyvinyl pyridine butyl quaternary ammonium loop construction.
Step 5：Polythiophene/polyvinyl pyridine butyl quaternary ammonium coil is placed in vacuum evaporation equipment, is adopted in coil head circumference
Silver electrode is prepared with vacuum deposition method, electrode is the film of thickness 200nm.Final obtain is based on polyaniline/polyvinyl pyridine
The electromagnetism chemical sensor of butyl quaternary ammonium coil.
Embodiment 6：
Step 1：
Ammonium persulfate 20mg, polystyrolsulfon acid 20mg are taken, is added in 100mL n-butanols, using magnetic force heating stirring 30
Minute, obtain ammonium persulfate/polystyrolsulfon acid solution.
Step 2：
Take 20mL ammonium persulfates/polystyrolsulfon acid solution and add in the syringe needle cavity of 3D printer, by default coil
Pattern prints ammonium persulfate/polystyrolsulfon acid loop construction, and printing speed is 1mm/min.
Step 3：
Ammonium persulfate/polystyrolsulfon acid coil is placed in 210 DEG C of steam-laden baking ovens and is heat-treated, water vapour
Vapour pressure is 0.65MPa, and processing time is 9 minutes.
Step 4：
Ammonium persulfate/polystyrolsulfon acid coil is placed in pyrrole monomer atmosphere, pyrrole monomer polymerize, polymerization temperature
Spend for 25 DEG C, obtain polypyrrole/polystyrolsulfon acid loop construction.
Step 5：Polypyrrole/polystyrolsulfon acid coil is placed in vacuum evaporation equipment, vacuum is used in coil head circumference
Evaporation coating method prepares copper electrode, and electrode is the film of thickness 200nm, and final obtain is based on polypyrrole/polystyrolsulfon acid coil
Electromagnetism chemical sensor.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause
This, all those of ordinary skill in the art without departing from disclosed spirit with being completed under technological thought
All equivalent modifications or change, should by the present invention claim be covered.
Claims (9)
1. a kind of preparation method of the electromagnetism chemical sensor based on conducting polymer, it is characterised in that include the following steps：
(1) oxidant containing ferric ion or over cure acid group is mixed with cationic polyelectrolyte, acquisition uniform oxidant/
High molecular polymer mixed liquor；
(2) oxidant/high molecular polymer mixed liquor is prepared as oxidant/high molecular polymer loop construction；
(3) oxidant/high molecular polymer loop construction is heat-treated, obtains oxidant/height with self-supporting effect
Molecularly Imprinted Polymer loop construction；
(4) above-mentioned oxidant/high molecular polymer coil is placed in monomer atmosphere and polymerize, obtain conducting polymer/height
Molecularly Imprinted Polymer loop construction；
(5) conducting polymer/high molecular polymer loop construction both ends are prepared into electrode, so that obtaining one kind is based on conducting polymer
The electromagnetism chemical sensor of thing.
2. the preparation method of the electromagnetism chemical sensor according to claim 1 based on conducting polymer, it is characterised in that：
Self-supporting effect refers to be not required extra substrate and frame to support, in its natural state can holding structure shape do not change
Feature.
3. the preparation method of the electromagnetism chemical sensor according to claim 1 based on conducting polymer, it is characterised in that：
The oxidant is ferric trichloride, toluenesulfonic acid iron, ammonium persulfate one kind therein.
4. the preparation method of the electromagnetism chemical sensor according to claim 1 based on conducting polymer, it is characterised in that：
The cationic polyelectrolyte is polystyrolsulfon acid, hydroxypropyl methyl cellulose, diallyl dimethyl ammoniumchloride, poly- third
Olefin(e) acid aqueous solution, polyvinyl pyridine butyl quaternary ammonium one kind therein.
5. the preparation method of the electromagnetism chemical sensor based on conducting polymer according to claim 1, it is special
Sign is：The method that loop construction is prepared in step (2) is 3D printing method.
6. the preparation method of the electromagnetism chemical sensor based on conducting polymer according to claim 1, it is special
Sign is：Heat treatment in step (3) for loop construction is placed in 195-210 DEG C of water vapor atmosphere, processing time for 5~
10 minutes.
7. the preparation method of the electromagnetism chemical sensor based on conducting polymer according to claim 1, it is special
Sign is：Monomer in step (4) is thiophene, 3,4- ethene dioxythiophenes, aniline, pyrroles conjugated polymers monomer in one
Kind.
8. the preparation method of the electromagnetism chemical sensor based on conducting polymer according to claim 1, its feature
It is：Electrode prepared by step (5) is gold, silver, the Copper thin film prepared using vacuum deposition method.
9. the electromagnetism chemical sensor based on conducting polymer that claim 1 to 8 any one preparation method obtains.
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| CN107917939B (en) | 2020-02-04 |
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