CN106290488A - Amino-functionalized carbon nanotube resistance type formaldehyde gas sensor and preparation method thereof - Google Patents
Amino-functionalized carbon nanotube resistance type formaldehyde gas sensor and preparation method thereof Download PDFInfo
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- CN106290488A CN106290488A CN201610828395.3A CN201610828395A CN106290488A CN 106290488 A CN106290488 A CN 106290488A CN 201610828395 A CN201610828395 A CN 201610828395A CN 106290488 A CN106290488 A CN 106290488A
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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
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
Abstract
The invention discloses an amino functionalized carbon nanotube resistance type formaldehyde gas sensor and a preparation method thereof. The gas-sensitive film is composed of amino-functionalized carbon nanotubes modified by tannic acid and polyethyleneimine. The gas sensor can detect formaldehyde gas at normal temperature, is insensitive to humidity, has strong anti-interference capability, high response sensitivity and quick response. The preparation method of the gas sensor is simple, easy to control and suitable for batch production, so that the gas sensor can be suitable for sensitive detection of formaldehyde in the fields of industrial production, process control, environment monitoring, modern agricultural production and the like.
Description
Technical field
The present invention relates to gas sensor domain, be specifically related to a kind of amino functional carbon nano tube resistor-type formaldehyde gas
Sensor and preparation method.
Background technology
Along with development intelligent, informationalized, the numerous areas of modern society, including environmental monitoring, commercial production,
Medical diagnosis and national defense and military etc., detection requirement real-time to gas in environment is more and more higher.Wherein formaldehyde gas is due to existence
Scope is wide, and the murder by poisoning to human body is big, and therefore the monitoring in real time of PARA FORMALDEHYDE PRILLS(91,95) is even more important.Development lightweight, portable formaldehyde gas
Body sensor will the life of the appreciable impact mankind. and at present, the main formaldehyde gas sensor used is that metal-oxide is partly led
Body (MOS) sensor and solid electrolyte (SE) sensor, but both of which needs to work at relatively high temperatures, power consumption is big,
Sensitivity is low, capacity of resisting disturbance is poor, uses inconvenience. and along with the development of nanotechnology, published in recent years is substantial amounts of relevant to be received
The research report of rice gas sensor, particularly CNT (CNTs) gas sensor have obtained substantially progress.
CNT has many advantages as gas sensor: specific surface area is big, the high adsorption capacity to gas；Often
Temperature is lower to be used, and reduces senor operating temperature；Chemical stability is good, and size is little.CNT is to NO2,SO2,NH3And O2Deng
Gas has preferable Detection results.But intrinsic CNT is due to self structure and the restriction of chemical property, can adsorb
Gaseous species very limited, be only limitted to several strong oxidizing property gas and strong reducing property gas, it is impossible to realize the detection of PARA FORMALDEHYDE PRILLS(91,95),
Thus be necessary carbon nano-tube modification.Carbon nano-tube modification is mainly organic decoration and inorganic doping.Inorganic doping is mainly
Introduce metal or metal-oxide on the carbon nanotubes.Although formaldehyde can preferably be detected, but cannot realize at room temperature
Lower detection.Organic decoration mainly introduces containing amido functional group by covalent bond or non-covalent bond normal direction carbon nano tube surface,
The interaction relying on amino and formaldehyde makes the resistance of gas sensor change thus realizes the detection of PARA FORMALDEHYDE PRILLS(91,95).But
The step that covalent bond method prepares amino functional carbon nano tube is comparatively laborious, and the conjugated structure of meeting destroying carbon nanometer tube, right
Its electric conductivity and sensing capabilities have adverse effect on.Although non-covalent bond method is convenient and simple, but due to amido functional group
And the force ratio between CNT is more weak, the most peeling-off when external condition changes, its stability is produced unfavorable shadow
Ring.Thus it is necessary that developing a kind of simple and effective new method prepares amino functional carbon nano tube resistor-type formaldehyde gas sensing
Device.
Summary of the invention
For overcoming the deficiencies in the prior art, the present invention provides a kind of amino functional carbon nano tube resistor-type formaldehyde gas to pass
Sensor and preparation method thereof.
Amino functional carbon nano tube resistor-type formaldehyde gas sensor preparation method, comprises the steps:
Form interdigital electrode by the method for silk screen printing, inkjet printing and photoetching on a flexible substrate, prepare and have
The flexible substrates of interdigital electrode；
CNT is added in the PBS of pH=7.5～9 ultrasonic 10～60min, and wherein carbon nanotube concentration is
0.5～2mg/ml.Then adding tannic acid in the suspension of above-mentioned CNT, tannic acid is the 0.5 of carbon nanotube mass
～2 times, the most ultrasonic 10～60min.The aqueous solution of polymine is slowly dropped to the suspension of tannic acid and CNT
In liquid, reacting 0.5～5h, obtain amido modified carbon nano-tube aqueous solutions, wherein the molecular weight of polymine can be 600
～10000, concentration is 1～10mg/ml, and the quality of polymine is 0.5～2 times of CNT.
By in the aqueous solution drop coating of the amido modified CNT of above-mentioned preparation to the flexible substrates with interdigital electrode,
Dried prepared amino functional carbon nano tube resistor-type formaldehyde gas sensor.
The air-sensitive film of the gas sensor of the present invention is by tannic acid and polymine non-covalent modified carbon nano-tube structure
Become, be to react cause tannic acid and polymine to exist by Michael's addition and the Schiff base of tannic acid with polymine
The in-situ cross-linked reaction of carbon nano tube surface, defines one layer of uniform tannic acid-polyethyleneimine amine copolymer in carbon nano tube surface
Thing realizes the surface modification to CNT, thus successfully amido functional group is incorporated into carbon nano tube surface.Tannic acid with
Macromolecular chain after polymine crosslinking can produce stronger repulsion and sterically hindered, it is possible to makes CNT preferably divide
It is dispersed in water, forms uniform dispersion liquid.CNT has bigger specific surface area, is conducive to improving sensitivity, simultaneously carbon
The amino of nanotube surface introducing and the interaction of formaldehyde so that the response of the CNT PARA FORMALDEHYDE PRILLS(91,95) of amino functional increases
By force.
Beneficial effects of the present invention is as follows:
(1) raw material tannic acid and polymine wide material sources, low price.
(2) surface amino groups functionalization one step of CNT completes, simple and fast；And carry out in aqueous, green ring
Protect.The present invention prepares that the method preparation method of gas sensor is simple, with low cost, be applicable to batch production.
(3) this gas sensor can detect by PARA FORMALDEHYDE PRILLS(91,95) gas at normal temperatures, insensitive to humidity, capacity of resisting disturbance
By force, and response sensitivity is high, and response is fast.
Accompanying drawing explanation
Fig. 1 is the amino functional carbon nano tube resistor-type formaldehyde gas sensor structural representation of the present invention；
Fig. 2 be the tannic acid polymine of the present invention carbon nano-tube modified transmission electron microscope picture, picture (a) is not
The transmission electron microscope of the CNT modified, picture (b) is the amine-modified amino functional carbon nano tube afterwards of tannic acid polyethyleneimine
Transmission electron microscope picture；
Fig. 3 is that the carbon nano-tube modified response to 50ppm formaldehyde of tannic acid polymine of the present invention and not adding is repaiied
The response to 50ppm formaldehyde of the CNT of decorations.
Detailed description of the invention
Embodiment 1
(1) forming 10 by inkjet printing in flexible substrate is the fork of 40 μm to interdigital width 40 μm, interdigital gap
Refer to gold electrode, prepare the flexible substrates with interdigital gold electrode；
(2) CNT of 10mg is added to fill ultrasonic 1h in the PBS of the pH=8.5 of 50ml；
(3) suspension of the CNT prepared adds the tannic acid of 50mg, and the most ultrasonic 1h；
(4) CNT prepared and the suspension of tannic acid drip the polymine (10mg/ml) of 5ml slowly,
The carbon nano-tube aqueous solutions of amino functional is obtained after reaction 1h；
(5) aqueous solution of the amido modified CNT of above-mentioned preparation is added drop-wise to the flexible base with interdigital gold electrode
, amino functional carbon nano tube resistor-type formaldehyde gas sensor is prepared at the end.
The carbon nanotube gas sensor PARA FORMALDEHYDE PRILLS(91,95) of amino functional prepared has and preferably detects performance.There is Fig. 3 can
Knowing, amino functional carbon nano tube resistor-type formaldehyde gas sensor prepared by the present invention at room temperature can detect with PARA FORMALDEHYDE PRILLS(91,95),
The formaldehyde of 50ppm there is is preferably response, and can reply.And the response of unmodified CNT PARA FORMALDEHYDE PRILLS(91,95) is less, table
The carbon nanotube gas sensor PARA FORMALDEHYDE PRILLS(91,95) of amino functional prepared by clear this method has preferable Detection results.
Embodiment 2
(1) forming 10 by inkjet printing on flexible matrix is the fork of 40 μm to interdigital width 40 μm, interdigital gap
Refer to gold electrode 2, prepare the flexible substrates with interdigital gold electrode；
(2) CNT of 10mg is added to fill ultrasonic 1h in the PBS of the pH=7 of 50ml；
(3) suspension of the CNT prepared adds the tannic acid of 50mg, and the most ultrasonic 1h；
(4) CNT prepared and the suspension of tannic acid drip the polymine (10mg/ml) of 5ml slowly,
The carbon nano-tube aqueous solutions of amino functional is obtained after reaction 1h；
(5) aqueous solution of the amido modified CNT of above-mentioned preparation is added drop-wise to the flexible base with interdigital gold electrode
, amino functional carbon nano tube resistor-type formaldehyde gas sensor is prepared at the end.
Comparative example 2 prepares amino functional carbon nano tube resistor-type formaldehyde gas sensor, to the response of gas relatively
Little less with the extent of reaction of polymine, so depositing on CNT mainly due to tannic acid in neutral conditions
Polymine the most less, thus Detection results is inconspicuous.
Embodiment 3
(1) being formed 5 to interdigital width 40 μm by silk screen printing on flexible substrate, interdigital gap is the interdigital gold of 40 μm
Electrode 2, prepares the flexible substrates with interdigital gold electrode；
(2) CNT of 10mg is added to fill ultrasonic 1h in the PBS of the pH=8.5 of 50ml；
(3) suspension of the CNT prepared adds the tannic acid of 50mg, and the most ultrasonic 1h；
(4) CNT prepared and the suspension of tannic acid drip the polymine (10mg/ml) of 5ml slowly,
The carbon nano-tube aqueous solutions of amino functional is obtained after reaction 1h；
(5) aqueous solution of the amido modified CNT of above-mentioned preparation is added drop-wise to the flexible base with interdigital gold electrode
, amino functional carbon nano tube resistor-type formaldehyde gas sensor is prepared at the end.
Embodiment 4
(1) forming 10 by inkjet printing on flexible substrate is the interdigital of 30 μm to interdigital width 30 μm, interdigital gap
Gold electrode 2, prepares the flexible substrates with interdigital gold electrode；
(2) CNT of 10mg is added to fill ultrasonic 1h in the PBS of the pH=8.5 of 50ml；
(3) suspension of the CNT prepared adds the tannic acid of 50mg, and the most ultrasonic 1h；
(4) CNT prepared and the suspension of tannic acid drip the polymine (10mg/ml) of 5ml slowly,
The carbon nano-tube aqueous solutions of amino functional is obtained after reaction 1h；
(5) aqueous solution of the amido modified CNT of above-mentioned preparation is added drop-wise to the flexible base with interdigital gold electrode
, amino functional carbon nano tube resistor-type formaldehyde gas sensor is prepared at the end.
Embodiment 5
(1) forming 10 by inkjet printing on flexible substrate is the interdigital of 40 μm to interdigital width 40 μm, interdigital gap
Silver electrode 2, prepares the flexible substrates with interdigital silver electrode；
(2) CNT of 10mg is added to fill ultrasonic 1h in the PBS of the pH=8.5 of 50ml；
(3) suspension of the CNT prepared adds the tannic acid of 50mg, and the most ultrasonic 1h；
(4) CNT prepared and the suspension of tannic acid drip the polymine (10mg/ml) of 5ml slowly,
The carbon nano-tube aqueous solutions of amino functional is obtained after reaction 1h；
(5) aqueous solution of the amido modified CNT of above-mentioned preparation is added drop-wise to the flexible base with interdigital silver electrode
, amino functional carbon nano tube resistor-type formaldehyde gas sensor is prepared at the end.
Embodiment 6
(1) forming 10 by inkjet printing on flexible substrate is the interdigital of 40 μm to interdigital width 40 μm, interdigital gap
Gold electrode 2, prepares the flexible substrates with interdigital gold electrode；
(2) CNT of 10mg is added to fill ultrasonic 1h in the PBS of the pH=8.5 of 50ml；
(3) suspension of the CNT prepared adds the tannic acid of 30mg, and the most ultrasonic 1h；
(4) CNT prepared and the suspension of tannic acid drip the polymine (10mg/ml) of 5ml slowly,
The carbon nano-tube aqueous solutions of amino functional is obtained after reaction 1h；
(5) aqueous solution of the amido modified CNT of above-mentioned preparation is added drop-wise to the flexible base with interdigital gold electrode
, amino functional carbon nano tube resistor-type formaldehyde gas sensor is prepared at the end.
The response that comparative example 6 prepares modified carbon nano-tube resistor-type formaldehyde gas sensor PARA FORMALDEHYDE PRILLS(91,95) is the least, main
If the amino content of the CNT of modification is less, thus the response of PARA FORMALDEHYDE PRILLS(91,95) is the least.
Embodiment 7
(1) forming 10 by inkjet printing on flexible substrate is the interdigital of 40 μm to interdigital width 40 μm, interdigital gap
Gold electrode 2, prepares the flexible substrates with interdigital gold electrode；
(2) CNT of 10mg is added to fill ultrasonic 1h in the PBS of the pH=8.5 of 50ml；
(3) suspension of the CNT prepared adds the tannic acid of 50mg, and the most ultrasonic 1h；
(4) CNT prepared and the suspension of tannic acid drip the polymine (10mg/ml) of 2ml slowly,
The carbon nano-tube aqueous solutions of amino functional is obtained after reaction 1h；
(5) aqueous solution of the amido modified CNT of above-mentioned preparation is added drop-wise to the flexible base with interdigital gold electrode
, amino functional carbon nano tube resistor-type formaldehyde gas sensor is prepared at the end.
The response that comparative example 7 prepares modified carbon nano-tube resistor-type formaldehyde gas sensor PARA FORMALDEHYDE PRILLS(91,95) is the least, says
The polymine of bright high level is also unfavorable for the response of modified carbon nano-tube PARA FORMALDEHYDE PRILLS(91,95).
Embodiment 8
(1) forming 10 by inkjet printing on flexible substrate is the interdigital of 40 μm to interdigital width 40 μm, interdigital gap
Gold electrode 2, prepares the flexible substrates with interdigital gold electrode；
(2) CNT of 10mg is added to fill ultrasonic 1h in the PBS of the pH=7 of 50ml；
(3) suspension of the CNT prepared adds the tannic acid of 50mg, and the most ultrasonic 1h；
(4) CNT prepared and the suspension of tannic acid drip the polymine (10mg/ml) of 5ml slowly,
The carbon nano-tube aqueous solutions of amino functional is obtained after reaction 10min；
(5) aqueous solution of the amido modified CNT of above-mentioned preparation is added drop-wise to the flexible base with interdigital gold electrode
, amino functional carbon nano tube resistor-type formaldehyde gas sensor is prepared at the end.
Claims (5)
1. an amino functional carbon nano tube resistor-type formaldehyde gas sensor, it is characterised in that: flexible substrates (1), interdigital
Electrode (2), air-sensitive film (3), lead-in wire (4), at the upper drop coating air-sensitive film (3) of above-mentioned flexible substrates and interdigital electrode (2), on
The air-sensitive film (3) stated is to be made up of the amino functional carbon nano tube after tannic acid and polyethyleneimine-modified.
A kind of amino functional carbon nano tube resistor-type formaldehyde gas sensor, it is characterised in that:
Described flexible substrate can be printing paper, polyethylene terephthalate (PET) film.
A kind of amino functional carbon nano tube resistor-type formaldehyde gas sensor, it is characterised in that:
Described interdigital electrode can be gold electrode, silver electrode, copper electrode and Graphene electrodes.
A kind of amino functional carbon nano tube resistor-type formaldehyde gas sensor, it is characterised in that:
Interdigital electrode is 5～10 to be the interdigital electrode of 30～60 μm to interdigital width 30～60 μm, interdigital gap.
5. an amino functional carbon nano tube resistor-type formaldehyde gas sensor preparation method, it is characterised in that include walking as follows
Rapid:
1) form interdigital electrode by the method for silk screen printing, inkjet printing and photoetching on a flexible substrate, prepare and there is fork
Refer to the flexible substrates of electrode；
2) CNT is added in the PBS of pH=7.5～9 ultrasonic 10～60min, and wherein carbon nanotube concentration is
0.5～2mg/ml；Then adding tannic acid in the suspension of above-mentioned CNT, tannic acid is the 0.5 of carbon nanotube mass
～2 times, the most ultrasonic 10～60min；The aqueous solution of polymine is added to slowly the suspension of tannic acid and CNT
In liquid, reacting 0.5～5h, obtain amino functional carbon nano-tube aqueous solutions, wherein the molecular weight of polymine can be 600
～10000, concentration is 1～10mg/ml, and the quality of polymine is 0.5～2 times of CNT；
3) by step 2) the aqueous solution drop coating of preparation-obtained amino functional carbon nano tube is to step 1) in there is interdigital electricity
In the flexible substrates of pole, obtain amino functional carbon nano tube resistor-type formaldehyde gas sensor after drying.
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| CN109060892A (en) * | 2018-06-26 | 2018-12-21 | 西安交通大学 | SF based on graphene composite material sensor array6Decompose object detecting method |
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| CN114002276A (en) * | 2021-08-25 | 2022-02-01 | 常州大学 | Resistance type humidity sensor based on carbon nano tube/titanium dioxide/polyethyleneimine composite membrane and preparation method thereof |
| CN114088778A (en) * | 2021-11-17 | 2022-02-25 | 湘潭大学 | High-repeatability film type PPB (pentatricopeptide repeats) formaldehyde gas sensor and preparation method thereof |
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| CN109060892A (en) * | 2018-06-26 | 2018-12-21 | 西安交通大学 | SF based on graphene composite material sensor array6Decompose object detecting method |
| CN109557142B (en) * | 2018-12-27 | 2021-07-09 | 东南大学 | Quick-response resistance type humidity sensor and preparation method and application thereof |
| CN109557142A (en) * | 2018-12-27 | 2019-04-02 | 东南大学 | A kind of resistance type humidity sensor of quick response and its preparation method and application |
| CN110632138A (en) * | 2019-11-01 | 2019-12-31 | 江南大学 | Interdigital electrode chip |
| CN110988075A (en) * | 2019-12-20 | 2020-04-10 | 肇庆学院 | Aminated multi-walled carbon nanotube electrochemical sensor and application thereof in detecting quercetin |
| CN114002276A (en) * | 2021-08-25 | 2022-02-01 | 常州大学 | Resistance type humidity sensor based on carbon nano tube/titanium dioxide/polyethyleneimine composite membrane and preparation method thereof |
| CN114088778A (en) * | 2021-11-17 | 2022-02-25 | 湘潭大学 | High-repeatability film type PPB (pentatricopeptide repeats) formaldehyde gas sensor and preparation method thereof |
| CN114088778B (en) * | 2021-11-17 | 2023-08-29 | 湘潭大学 | High-repeatability film type PPB-level formaldehyde gas sensor and preparation method thereof |
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