CN109030576A - A kind of nitrogen dioxide gas electronic sensor material and preparation method - Google Patents
A kind of nitrogen dioxide gas electronic sensor material and preparation method Download PDFInfo
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- CN109030576A CN109030576A CN201810683446.7A CN201810683446A CN109030576A CN 109030576 A CN109030576 A CN 109030576A CN 201810683446 A CN201810683446 A CN 201810683446A CN 109030576 A CN109030576 A CN 109030576A
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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
Abstract
The invention belongs to the technical field of sensor, a kind of nitrogen dioxide gas electronic sensor material and preparation method are provided.This method modifies nano zine oxide with polystyrolsulfon acid, and pyrrole monomer is made to carry out in-situ polymerization in zinc oxide surface, the aqueous solution of zinc oxide/Pt/Polypyrrole composite material is made, is then spin coated onto the surface in interdigital gold electrode and drying, nitrogen dioxide gas electronic sensor material is made.It is compared with the traditional method, the gas sensing material of preparation of the invention, the zinc oxide for the obtaining stable uniform/Pt/Polypyrrole composite material aqueous dispersions obtained by the zinc oxide surface in-situ polymerization pyrroles modified in polystyrolsulfon acid, significantly improve the composite performance of zinc oxide and polypyrrole, ensure the consistency and stability of gas sensor, nitrogen dioxide gas sensor sensitivity is improved, can be effectively used for the detection of nitrogen dioxide gas.
Description
Technical field
The invention belongs to the technical field of sensor, a kind of nitrogen dioxide gas electronic sensor material and preparation side are provided
Method.
Background technique
Since 20 end of the century mankind enter information-intensive society, the activities of people are handed over acquisition of information and information
It is changed to center, the new period of high speed development is also entered as the basis of information technology and the sensor technology of one of three big pillars.
With continuous improvement of people's living standards and to the pay attention to day by day of environmental protection, to various toxic, pernicious gas detections, to atmosphere
Pollution, the monitoring of industrial waste gas and the detection to food and habitation environment quality, propose higher want to gas sensor
It asks.
Gas sensor is that a kind of be converted into the information such as the composition of gas, concentration can be by personnel, instrument and meter, calculating
The device gas sensor for the information that machine etc. utilizes is generally categorized as one kind of chemical sensor, although this sort out not necessarily section
It learns.Specifically include that semiconductor gas sensor, electrochemical gas sensor, catalytic combustion method gas sensor, heat-conducted gas
Sensor, infrared gas sensor, solid-state electrolyte gas sensor etc..
At present the metal oxide semiconductor material of gas sensor material oneself tend to maturing, current work is main
There are two direction: being using chemical modification method of modifying, be doped, be modified and surface modification to existing gas sensitization membrane material
Deng processing, and film-forming process is improved and optimized, improves the stability and selectivity of gas sensor；It is to develop newly
Gas sensitization membrane material, such as compound and mixed type Semiconductor gas sensors material, macromolecule gas sensitive, so that these new materials
There is highly sensitive, highly selective, high stability to gas with various.Due to interdigital electrode to the film resistor being coated on,
Change of electrolyte response is extremely sensitive, therefore the resistor-type based on interdigital electrode, capacitive gas sensor are like the mushrooms after rain
It emerges in large numbers.
Certain effect has been achieved in terms of sensor technology, especially gas sensing material both at home and abroad at present.Wherein ancestral
Bai Yi et al. has invented a kind of nitrogen dioxide sensor based on titanium dioxide/graphene and preparation method (Chinese invention patent
Application number 201310234385.3), which is by ceramic bases, electrode, titanium dioxide/graphene composite material, heating
Device and thermocouple and signal processing part are grouped as, and the use of titanium dioxide/graphene composite material are NO2Gas-sensitive Functional Materials lead to
Cross measurement NO2The variation of material resistance reaches to NO when being adsorbed to material surface2The purpose of sensing；Measuring signal is sensor electricity
Voltage, curent change in resistive or thus caused circuit；The sensor have operating temperature is low, temperature-responsive range is wide,
High sensitivity, detection limit for height, response time short feature.In addition, Fu Tiexiang has invented an a kind of nitrogen dioxide gas sensor
And preparation method thereof (Chinese invention patent application number 201410633610.5), the sensor composition include: ceramics pipe outer, if
In a pair of metal electrodes and metal extraction wire in ceramics pipe outer and it is sprayed on metal electrode and ceramics pipe outer
Gas sensitive layer；Wherein gas sensitive layer is by complex [Fe(bipyO2) Cl2] Cl composition；The preparation method is as follows: by anhydrous
FeCl3With bipyO2Synthetic compound [the Fe(bipyO in the DMF of boiling2) Cl2]Cl.Take [Fe(bipyO2) Cl2] Cl solid grinds
Mill 2 hours, it is then ultrasonic evenly dispersed in deionized water, 0.1% polyvinyl alcohol adhesive is added；Gained colloidal sol is sprayed
It is 3 hours dry onto interdigital electrode and insulation tube；The sensor has responsiveness good, response and restores fast, non-sintered, can be
The advantages of working at room temperature.
Stablize as it can be seen that gas sensing material in the prior art, especially nitrogen dioxide gas electronic sensor material exist
The disadvantages of property is poor, and sensitivity is not high, and then affect the further development and application of gas sensing material.
Summary of the invention
In response to this, it is proposed that a kind of nitrogen dioxide gas electronic sensor material and preparation method, significantly improve
The consistency and stability of nitrogen dioxide gas sensor, and high sensitivity.
To achieve the above object, specific technical solution of the present invention is as follows:
A kind of preparation method of nitrogen dioxide gas electronic sensor material is modified nano zine oxide with polystyrolsulfon acid, and is made
Pyrrole monomer zinc oxide surface carry out in-situ polymerization, be made zinc oxide/Pt/Polypyrrole composite material aqueous solution, be then spin coated onto
Nitrogen dioxide gas electronic sensor material is made in the surface of interdigital gold electrode and drying, and specific step is as follows for preparation:
(1) it using interdigital gold electrode as the working electrode in three-electrode system, is placed in sulfuric acid solution, carries out Electrochemical Scanning,
Until the oxide on surface is cleaned, then it is dried for standby；
(2) aqueous solution for configuring polystyrolsulfon acid, then nano zine oxide is added in polystyrolsulfon acid aqueous solution, ultrasound
The mix moisture dispersion liquid of polystyrolsulfon acid and zinc oxide is made in dispersion；
(3) pyrrole monomer is evaporated under reduced pressure, is then added in mix moisture dispersion liquid made from step (2), ammonium persulfate water is added
Solution, being stirred makes pyrrole monomer that polymerization reaction occur in surface of nanometer zinc oxide, and zinc oxide/Pt/Polypyrrole composite material is made
Aqueous solution；
(4) zinc oxide/Pt/Polypyrrole composite material aqueous solution made from step (3) is spun on to the surface of interdigital gold electrode, is done
Dry formation sensitive membrane, as nitrogen dioxide gas electronic sensor material.
Preferably, the concentration of step (1) described sulfuric acid solution is 1mol/L.
Preferably, the potential range of step (1) described Electrochemical Scanning is -0.1 ~ 1.2V.
Preferably, the temperature of step (1) described drying is 120 ~ 140 DEG C, and the time is 40 ~ 60min.
Preferably, in the mix moisture dispersion liquid of step (2) polystyrolsulfon acid and zinc oxide, polystyrolsulfon acid 5 ~
10 parts by weight, 25 ~ 30 parts by weight of zinc oxide, 60 ~ 70 parts by weight of water.
Preferably, the supersonic frequency of step (2) described ultrasonic disperse is 40 ~ 60kHz, and the time is 20 ~ 30min.
Preferably, the parts by weight of step (3) each raw material are 30 ~ 40 parts by weight of pyrrole monomer, 5 ~ 10 weight of ammonium persulfate
Measure 50 ~ 65 parts by weight of mix moisture dispersion liquid of part, polystyrolsulfon acid and zinc oxide.
Preferably, the rotation speed of step (4) described spin coating is 3000 ~ 3500r/min, and rotational time is 18 ~ 22s.
Preferably, step (4) is described dry using heater-type ceramic infrared drying machine, and drying time is 10 ~ 15min.
Conventional zinc oxide/polypyrrole composite sensitive film preparation method is that zinc oxide and polypyrrole progress is simply total
It is mixed, and the present invention creatively introduces polystyrolsulfon acid during the preparation process, on the one hand to the surface of nano zine oxide into
Row modification, improves the water dispersion of zinc oxide, and on the other hand, polystyrolsulfon acid serves as the dopant of polypyrrole, induces pyrrole
It coughs up monomer and carries out in-situ polymerization on the surface of nano zine oxide, thus the zinc oxide made/Pt/Polypyrrole composite material water dispersion
Liquid is more uniform and stablizes, and improves the consistency and stability of gas sensor.As it can be seen that the introducing of polystyrolsulfon acid, favorably
In promoting nano zine oxide and polypyrrole to generate good synergistic effect, nitrogen dioxide gas sensor sensitivity is improved.
The present invention also provides a kind of nitrogen dioxide gas electronic sensor materials that above-mentioned preparation method is prepared.
The preparation method of the gas sensing material is to modify nano zine oxide with polystyrolsulfon acid, and pyrrole monomer is made to exist
Zinc oxide surface carries out in-situ polymerization, and the aqueous solution of zinc oxide/Pt/Polypyrrole composite material is made, is then spin coated onto interdigital gold electrode
Surface and drying, be made nitrogen dioxide gas electronic sensor material.It is compared with the traditional method, the gas of preparation of the invention passes
Feel material, obtains the oxidation of stable uniform by what the zinc oxide surface in-situ polymerization pyrroles modified in polystyrolsulfon acid obtained
Zinc/Pt/Polypyrrole composite material aqueous dispersions, hence it is evident that improve the composite performance of zinc oxide and polypyrrole, it is ensured that gas sensor
Consistency and stability improve nitrogen dioxide gas sensor sensitivity, can be effectively used for the detection of nitrogen dioxide gas.
The present invention provides a kind of nitrogen dioxide gas electronic sensor material and preparation methods, compared with prior art,
Prominent feature and excellent effect are:
1. gas sensing material prepared by the present invention, can be effectively used for the detection of nitrogen dioxide gas.
2. preparation method of the invention, zinc oxide/Pt/Polypyrrole composite material of preparation is by repairing in polystyrolsulfon acid
What the zinc oxide surface in-situ polymerization pyrroles of decorations obtained, rather than simple physical blending, accordingly ensure that composite material is excellent
Anisotropic energy.
3. preparation method of the invention obtains zinc oxide/polypyrrole of stable uniform by the way that polystyrolsulfon acid is added
Aqueous nancomposite dispersion liquid, hence it is evident that improve the composite performance of zinc oxide and polypyrrole, it is ensured that the consistency of gas sensor and
Stability improves nitrogen dioxide gas sensor sensitivity.
Specific embodiment
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
Using interdigital gold electrode as the working electrode in three-electrode system, it is placed in the sulfuric acid solution that concentration is 1mol/L, in electricity
Position range is to carry out Electrochemical Scanning under 0.5V, until the oxide on surface is cleaned, then in 132 DEG C of drying 48min
It is spare；Then 7kg polystyrolsulfon acid is added in 66kg water and is configured to solution, polyphenyl then is added in 27kg nano zine oxide
In vinyl sulfonic acid aqueous solution, disperses 26min in the case where frequency is the ultrasonic wave of 52kHz, polystyrolsulfon acid and zinc oxide is made
Mix moisture dispersion liquid；Then 36kg pyrrole monomer is evaporated under reduced pressure, is then added in 57kg mix moisture dispersion liquid, 7kg mistake is added
Ammonium sulfate is stirred generation polymerization reaction, and the aqueous solution of zinc oxide/Pt/Polypyrrole composite material is made；Finally aqueous solution is revolved
It is applied to the surface of interdigital gold electrode, rotation speed 3300r/min, rotational time 21s are dry using heater-type ceramic infrared
The dry 13min of dry machine forms sensitive membrane, as nitrogen dioxide gas electronic sensor material.
Test method:
(1) stability test: gas sensing material produced by the present invention is used for gas sensor, experimental condition is room temperature, often
Wet, element is in normal operating conditions, and senor operating temperature is 300 DEG C, operating voltage 10V；Certainly using gas sensor
Dynamic test macro, test nitrogen dioxide gas pass first into pure air 20min before, and flow 800mL/min is then passed to
Nitrogen dioxide gas 5min, then logical pure air 20min clean test chamber, and sensor is made to be restored to the baseline value in air；Into
Row iterative cycles 100 times, 200 times and 300 times tests；Using difference comparsion method, leads to and extract sensor in nitrogen dioxide gas
Voltage value, compare former and later two circulation difference, difference is smaller, and sensor is more stable.Wherein, | Δ Vg| in tested gas
Measurement voltage head and the tail circulation absolute value of the difference.
(2) sensitivity test: gas sensing material produced by the present invention is used for gas sensor, experimental condition is normal
Wet, temperature is 20 DEG C, and element is in normal operating conditions, and equipment is gas sensitivity tester, in 2ppm content of nitrogen dioxide
Nitrogen dioxide gas test is carried out under atmosphere, output voltage changing value, as sensitivity when concentration changes 1ppm.
The data obtained is as shown in table 1.
Embodiment 2
Using interdigital gold electrode as the working electrode in three-electrode system, it is placed in the sulfuric acid solution that concentration is 1mol/L, in electricity
Position range is to carry out Electrochemical Scanning under -0.1V, until the oxide on surface is cleaned, then in 120 DEG C of drying 60min
It is spare；Then 5kg polystyrolsulfon acid is added in 70kg water and is configured to solution, polyphenyl then is added in 25kg nano zine oxide
In vinyl sulfonic acid aqueous solution, disperses 30min in the case where frequency is the ultrasonic wave of 40kHz, polystyrolsulfon acid and zinc oxide is made
Mix moisture dispersion liquid；Then 30kg pyrrole monomer is evaporated under reduced pressure, is then added in 65kg mix moisture dispersion liquid, 5kg mistake is added
Ammonium sulfate is stirred generation polymerization reaction, and the aqueous solution of zinc oxide/Pt/Polypyrrole composite material is made；Finally aqueous solution is revolved
It is applied to the surface of interdigital gold electrode, rotation speed 3000r/min, rotational time 22s are dry using heater-type ceramic infrared
The dry 10min of dry machine forms sensitive membrane, as nitrogen dioxide gas electronic sensor material.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Embodiment 3
Using interdigital gold electrode as the working electrode in three-electrode system, it is placed in the sulfuric acid solution that concentration is 1mol/L, in electricity
Position range is to carry out Electrochemical Scanning under 0.3V, until the oxide on surface is cleaned, then in 125 DEG C of drying 55min
It is spare；Then 6kg polystyrolsulfon acid is added in 68kg water and is configured to solution, polyphenyl then is added in 26kg nano zine oxide
In vinyl sulfonic acid aqueous solution, disperses 28min in the case where frequency is the ultrasonic wave of 45kHz, polystyrolsulfon acid and zinc oxide is made
Mix moisture dispersion liquid；Then 32kg pyrrole monomer is evaporated under reduced pressure, is then added in 61kg mix moisture dispersion liquid, 7kg mistake is added
Ammonium sulfate is stirred generation polymerization reaction, and the aqueous solution of zinc oxide/Pt/Polypyrrole composite material is made；Finally aqueous solution is revolved
It is applied to the surface of interdigital gold electrode, rotation speed 3100r/min, rotational time 21s are dry using heater-type ceramic infrared
The dry 11min of dry machine forms sensitive membrane, as nitrogen dioxide gas electronic sensor material.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Embodiment 4
Using interdigital gold electrode as the working electrode in three-electrode system, it is placed in the sulfuric acid solution that concentration is 1mol/L, in electricity
Position range is to carry out Electrochemical Scanning under 1.2V, until the oxide on surface is cleaned, then in 140 DEG C of drying 40min
It is spare；Then 10kg polystyrolsulfon acid is added in 60kg water and is configured to solution, then 30kg nano zine oxide is added poly-
In styrene sulfonic acid aqueous solution, disperses 20min in the case where frequency is the ultrasonic wave of 60kHz, polystyrolsulfon acid and zinc oxide is made
Mix moisture dispersion liquid；Then 40kg pyrrole monomer is evaporated under reduced pressure, is then added in 50kg mix moisture dispersion liquid, 10kg is added
Ammonium persulfate is stirred generation polymerization reaction, and the aqueous solution of zinc oxide/Pt/Polypyrrole composite material is made；Finally by aqueous solution
It is spun on the surface of interdigital gold electrode, rotation speed 3500r/min, rotational time 18s, using heater-type ceramic infrared
The dry 15min of drying machine forms sensitive membrane, as nitrogen dioxide gas electronic sensor material.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Embodiment 5
Using interdigital gold electrode as the working electrode in three-electrode system, it is placed in the sulfuric acid solution that concentration is 1mol/L, in electricity
Position range is carries out Electrochemical Scanning under 1V, until the oxide on surface is cleaned, it is then standby in 135 DEG C of drying 45min
With；Then 9kg polystyrolsulfon acid is added in 63kg water and is configured to solution, polyphenyl second then is added in 28kg nano zine oxide
In alkene sulfonic acid aqueous solution, disperses 23min in the case where frequency is the ultrasonic wave of 55kHz, the mixed of polystyrolsulfon acid and zinc oxide is made
Heshui dispersion liquid；Then 38kg pyrrole monomer is evaporated under reduced pressure, is then added in 54kg mix moisture dispersion liquid, 8kg over cure is added
Sour ammonium is stirred generation polymerization reaction, and the aqueous solution of zinc oxide/Pt/Polypyrrole composite material is made；Finally by aqueous solution spin coating
In the surface of interdigital gold electrode, rotation speed 3400r/min, rotational time 19s are dry using heater-type ceramic infrared
The dry 14min of machine forms sensitive membrane, as nitrogen dioxide gas electronic sensor material.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Embodiment 6
Using interdigital gold electrode as the working electrode in three-electrode system, it is placed in the sulfuric acid solution that concentration is 1mol/L, in electricity
Position range is to carry out Electrochemical Scanning under 0.6V, until the oxide on surface is cleaned, then in 130 DEG C of drying 50min
It is spare；Then 8kg polystyrolsulfon acid is added in 64kg water and is configured to solution, polyphenyl then is added in 28kg nano zine oxide
In vinyl sulfonic acid aqueous solution, disperses 25min in the case where frequency is the ultrasonic wave of 50kHz, polystyrolsulfon acid and zinc oxide is made
Mix moisture dispersion liquid；Then 35kg pyrrole monomer is evaporated under reduced pressure, is then added in 57kg mix moisture dispersion liquid, 8kg mistake is added
Ammonium sulfate is stirred generation polymerization reaction, and the aqueous solution of zinc oxide/Pt/Polypyrrole composite material is made；Finally aqueous solution is revolved
It is applied to the surface of interdigital gold electrode, rotation speed 3250r/min, rotational time 20s are dry using heater-type ceramic infrared
The dry 12min of dry machine forms sensitive membrane, as nitrogen dioxide gas electronic sensor material.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Comparative example 1
In gas sensing material preparation process, it is not added with polystyrolsulfon acid, other preparation conditions and embodiment 6 are consistent.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Table 1:
Claims (10)
1. a kind of preparation method of nitrogen dioxide gas electronic sensor material, which is characterized in that received with polystyrolsulfon acid modification
Rice zinc oxide, and pyrrole monomer is made to carry out in-situ polymerization in zinc oxide surface, the water-soluble of zinc oxide/Pt/Polypyrrole composite material is made
Liquid is then spin coated onto the surface in interdigital gold electrode and drying, and nitrogen dioxide gas electronic sensor material, the specific step of preparation is made
It is rapid as follows:
(1) it using interdigital gold electrode as the working electrode in three-electrode system, is placed in sulfuric acid solution, carries out Electrochemical Scanning,
Until the oxide on surface is cleaned, then it is dried for standby；
(2) aqueous solution for configuring polystyrolsulfon acid, then nano zine oxide is added in polystyrolsulfon acid aqueous solution, ultrasound
The mix moisture dispersion liquid of polystyrolsulfon acid and zinc oxide is made in dispersion；
(3) pyrrole monomer is evaporated under reduced pressure, is then added in mix moisture dispersion liquid made from step (2), ammonium persulfate water is added
Solution, being stirred makes pyrrole monomer that polymerization reaction occur in surface of nanometer zinc oxide, and zinc oxide/Pt/Polypyrrole composite material is made
Aqueous solution；
(4) zinc oxide/Pt/Polypyrrole composite material aqueous solution made from step (3) is spun on to the surface of interdigital gold electrode, is done
Dry formation sensitive membrane, as nitrogen dioxide gas electronic sensor material.
2. a kind of preparation method of nitrogen dioxide gas electronic sensor material according to claim 1, it is characterised in that: step
(1) concentration of the sulfuric acid solution is 1mol/L.
3. a kind of preparation method of nitrogen dioxide gas electronic sensor material according to claim 1, it is characterised in that: step
(1) potential range of the Electrochemical Scanning is -0.1 ~ 1.2V.
4. a kind of preparation method of nitrogen dioxide gas electronic sensor material according to claim 1, it is characterised in that: step
(1) temperature of the drying is 120 ~ 140 DEG C, and the time is 40 ~ 60min.
5. a kind of preparation method of nitrogen dioxide gas electronic sensor material according to claim 1, it is characterised in that: step
(2) in the mix moisture dispersion liquid of the polystyrolsulfon acid and zinc oxide, 5 ~ 10 parts by weight of polystyrolsulfon acid, zinc oxide 25 ~
30 parts by weight, 60 ~ 70 parts by weight of water.
6. a kind of preparation method of nitrogen dioxide gas electronic sensor material according to claim 1, it is characterised in that: step
(2) supersonic frequency of the ultrasonic disperse is 40 ~ 60kHz, and the time is 20 ~ 30min.
7. a kind of preparation method of nitrogen dioxide gas electronic sensor material according to claim 1, it is characterised in that: step
(3) parts by weight of each raw material are, 30 ~ 40 parts by weight of pyrrole monomer, 5 ~ 10 parts by weight of ammonium persulfate, polystyrolsulfon acid and
50 ~ 65 parts by weight of mix moisture dispersion liquid of zinc oxide.
8. a kind of preparation method of nitrogen dioxide gas electronic sensor material according to claim 1, it is characterised in that: step
(4) rotation speed of the spin coating is 3000 ~ 3500r/min, and rotational time is 18 ~ 22s.
9. a kind of preparation method of nitrogen dioxide gas electronic sensor material according to claim 1, it is characterised in that: step
(4) described dry using heater-type ceramic infrared drying machine, drying time is 10 ~ 15min.
10. the nitrogen dioxide gas electronic sensor material that any one of claim 1 ~ 9 preparation method is prepared.
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| CN103235010A (en) * | 2013-04-15 | 2013-08-07 | 江南大学 | Water dispersible polyaniline/carbon nanotube composite resistive type film gas-sensitive element and preparation method thereof |
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Application publication date: 20181218 |