CN107764871A - To NOXPPy/SnO with high selectivity2Nanotube composite air-sensitive material - Google Patents
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Abstract
The present invention proposes a kind of to NOXPPy/SnO with high selectivity2Nanotube composite air-sensitive material, solve in the prior art gas sensitive in the range of low-temperature working to NOXPoor selectivity, and the problem of sensitivity is relatively low.The present invention is prepared in the following manner:(1)Configure SnO2The precursor solution of nanofiber;(2)Electrostatic spinning prepares PVP composite nano fibers;(3)Calcining prepares SnO2Nanotube fibers;(4)Prepare PPy/SnO2Nanometer tube composite materials.The gas sensitive that the present invention obtains is to NOXSensitivity be common SnO2Three times, and to H2S、NH3, acetone, absolute ethyl alcohol sensitivity not increase even have obvious reduction, improve to NOXSelectivity, be particularly suitable for being NOXGas sensor.
Description
Technical field
The present invention relates to a kind of gas sensitive, and in particular to a kind of to NOxSelective gas sensitive.
Background technology
With industrialized fast development, NO, NO2Deng oxynitrides(NOX)Pollution problem become increasingly conspicuous, NOXHave
It is toxic, and acid rain, eutrophication and stratospheric ozone layer leak etc. also all with NOxGas is relevant.NO is combined blood red simultaneously
The ability of albumen is also stronger than carbon monoxide, it is easier to causes human body anoxia, NO is easily oxidized into NO in atmosphere2, and NO2
There is strong impulse effect to respiratory tract, lung damage even pulmonary edema, therefore to NO can be caused when seriousXThe real-time prison of gas
Survey very urgent.
Measure NO at presentxMethod mainly using the chromatography of ions, gas chromatography etc., these methods need expensive instrument
Device equipment, sampling analysis need to expend longer time, it is difficult to realize to NOXLive continuous monitoring.Oxide semiconductor gas
Dependent sensor obtains because with series of advantages such as simple in construction, cheap, easy to use and easy realization miniaturizations
Develop rapidly, but oxide semiconductor is easily affected by temperature and drifted about there is also output characteristics simultaneously, operating temperature is high, selection
The shortcomings of property difference.Conducting polymer gas sensitive can be deposited on various substrates, and can be by selecting different big points
Subchain structure, and being modified to it, so as to obtain different chemical-sensitive performances, improve its sensitivity to gas response and
Selectivity, it is most important that it can work at room temperature, but there is also easily by ambient temperature and humidity for conducting polymer air-sensitive film
Influence, long-time stability are poor and the shortcomings of poor selectivity.By organic polymer conducting polymer and Nano semiconductor metal oxygen
The organic/inorganic semiconductor composite that compound combines to form, combine the respective excellent of conducting polymer and oxide semiconductor
Point, many excellent performances of material are imparted in terms of air-sensitive, can be greatly improved to NOxThe low temperature detectivity of gas.Together
When, 1-dimention nano tubular construction is made in gas sensitive, big specific surface area can be obtained, is more beneficial for improving the gas sensing property of material
Energy.
The content of the invention
The present invention proposes a kind of to NOXPPy/SnO with high selectivity2Nanotube composite air-sensitive material, is solved existing
In technology gas sensitive in the range of low-temperature working to NOXPoor selectivity, and the problem of sensitivity is relatively low.
It is a kind of to NOXPPy/SnO with high selectivity2Nanotube composite air-sensitive material, it is to prepare in the following manner
's:
(1)Configure SnO2The precursor solution of nanofiber:0.7-1.2g PVP is added in 8-13ml absolute ethyl alcohol and stirred
Mix 1-3h and obtain solution A, by 0.6-1.2 g SnCl2•2H2O is added to stirring 1-2h in 3-8ml DMF and obtains solution B, so
Solution A is poured into B solution afterwards, and stirs 2-4h and obtains transparent precursor solution;
(2)Electrostatic spinning prepares PVP composite nano fibers:By step(1)In precursor solution be fitted into syringe, use is quiet
Electrospinning carries out spinning and obtains PVP composite nano fibers;
(3)Calcining prepares SnO2Nanotube fibers:By step(2)In PVP composite nano fibers be put into annealing furnace, in air
Calcination processing is carried out in atmosphere, from room temperature to 550~700 DEG C, programming rate is not less than 10 DEG C/min, calcination time 1.5
~10h, room temperature is naturally cooled to body of heater afterwards, obtain SnO2Nanotube fibers;
(4)Prepare PPy/SnO2Nanometer tube composite materials:By 5-25mg surfactant and 0.03-0.2g SnO2Nanowire
Dimension is added separately in the 50ml aqueous solution, and 1-3h is stirred at room temperature, and is added 1.5-8 μ l Py monomers afterwards and is stirred 0.5-2h, most
The FeCl that concentration is 0.1mol/L is added afterwards3Aqueous solution 1-5ml, reacted under stirring, carry out filtering after 2-7h and clear
Wash, obtain PPy/SnO2Nanometer tube composite materials.
Step(2)The condition of middle electrostatic spinning technique is:Direct current spinning voltage is 5~16 kV, and nozzle and receiver are consolidated
It is 10~25cm to change distance.
The surfactant is lauryl sodium sulfate or neopelex.
Step(1)In be by 1g PVP be added in 10ml absolute ethyl alcohol stir 2h obtain solution A, by 0.8 g's
SnCl2•2H2O be added to 4ml DMF stirring 2h obtain solution B, then solution A is poured into B solution, and stir 2h obtain it is transparent
Precursor solution.
Step(1)In be by 0.8g PVP be added in 9ml absolute ethyl alcohol stir 2h obtain solution A, by 1.2 g's
SnCl2•2H2The DMF stirrings 2.5h that O is added to 5ml obtains solution B, and then solution A is poured into B solution, and is stirred 2h and obtained
Bright precursor solution.
The gas sensitive that the present invention obtains is to NOXSensitivity be common SnO2Three times, and to H2S、NH3, acetone, nothing
The sensitivity of water-ethanol, which does not increase, even has obvious reduction, improves to NOXSelectivity, be particularly suitable for being NOXGas sensitive element
Part.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is the transmission electron microscope picture of the present invention.
Fig. 2 is PPy/SnO2Nanometer tube composite materials and SnO2To NOXSelective comparison diagram.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other under the premise of creative work is not paid
Embodiment, belong to the scope of protection of the invention.
It is a kind of to NOXPPy/SnO with high selectivity2Nanotube composite air-sensitive material, it is to prepare in the following manner
's:
(1)Configure SnO2The precursor solution of nanofiber:0.7-1.2g PVP is added in 8-13ml absolute ethyl alcohol and stirred
Mix 1-3h and obtain solution A, by 0.6-1.2 g SnCl2•2H2O(Stannous chloride)Stirring 1-2h in 3-8ml DMF is added to obtain
To solution B, then solution A is poured into B solution, and stirs 2-4h and obtains transparent precursor solution;
(2)Electrostatic spinning prepares PVP composite nano fibers:By step(1)Middle precursor solution is fitted into syringe, using electrostatic
Spining technology carries out spinning and obtains PVP composite nano fibers;
(3)Calcining prepares SnO2Nanotube fibers:By step(2)Obtained PVP composite nano fibers are put into annealing furnace, in sky
Calcination processing is carried out in atmosphere, from room temperature to 550~700 DEG C, programming rate is not less than 10 DEG C/min, and calcination time is
1.5~10h, room temperature is naturally cooled to body of heater afterwards, obtain SnO2Nanotube fibers;
(4)Prepare PPy/SnO2Nanometer tube composite materials:By 5-20mg surfactant and 0.03-0.2g SnO2Nanowire
Dimension is added separately in the 50ml aqueous solution, and 1-3h is stirred at room temperature, and is added 1.5-8 μ l Py monomers afterwards and is stirred 0.5-2h, most
The FeCl that concentration is 0.1mol/L is added afterwards3Aqueous solution 1-5ml, it is poly- that liquid phase chemical oxidation is carried out in the case where being kept stirring for
Reaction is closed, is filtered and is cleaned after 2-7h, obtains PPy/SnO2Nanometer tube composite materials.
Preferably, step(2)The technical conditions of electrostatic spinning are:Direct current spinning voltage is 5~16kV, nozzle and receiver
Solidification distance be 10~25cm.
Wherein, the surfactant is lauryl sodium sulfate or neopelex.
Illustrate the preparation method and advantage of the present invention below in conjunction with specific embodiment:
Embodiment 1:1g PVP (polyvinylpyrrolidone) is added to stirring 2h in 10ml absolute ethyl alcohol and obtains solution A, will
0.8 g stannous chloride(SnCl2•2H2O)It is added in 4ml DMF(DMF)Stirring 2h obtains solution B,
Then solution A is poured into B solution, and stirs 2h and obtain transparent precursor solution.
Spinning is carried out using electrostatic spinning technique, it is 12kV to set direct current spinning voltage, the solidification of nozzle and receiver away from
From for 15cm, the PVP composite nano fibers containing presoma are obtained.PVP composite nano fibers are put into annealing furnace, in air atmosphere
Middle carry out calcination processing, from room temperature to 600 DEG C, programming rate is 10 DEG C/min, calcination time 3h, afterwards with body of heater from
Room temperature is so cooled to, obtains SnO2Nanotube fibers.
By 20mg lauryl sodium sulfate and 0.05g SnO2Hollow Nano fiber in use is added separately in the 50ml aqueous solution
3h is stirred at room temperature, adds 2.585 μ l Py monomers afterwards and stirs 1h, be eventually adding 1.1ml FeCl3The aqueous solution(Concentration is
0.1mol/L), liquid phase chemical oxidative polymerization is carried out in the case where being kept stirring for, is filtered and is cleaned after 4h, is obtained
PPy/SnO2Nanometer tube composite materials.
In the present embodiment, lauryl sodium sulfate can also be replaced with neopelex.
PPy/SnO in the present embodiment2Nanometer tube composite materials TEM results are as shown in figure 1, utilize liquid phase chemical oxidation polymerization
PPy prepared by method is coated on SnO2The surface of nanotube forms core shell structure.The gas sensing that gained composite is made
Device has carried out air-sensitive performance test, is the resistance in air using formula S=(Ra-Rg)/Rg, Ra, after Rg is is passed through test gas
Resistance, to 5ppm NH at 120 DEG C3、H2S, CO, NOx and 500ppm absolute ethyl alcohol, methanol, acetone carry out air-sensitive survey
Examination.As shown in Figure 2, it can be seen that relative to SnO2Nanotube fibers, PPy/SnO in the present embodiment2Nanometer tube composite materials pair
NOXSensitivity improve about 3 times, and the sensitivity to other gases does not significantly improve, and the present embodiment is to H2S, anhydrous second
Alcohol, the sensitivity of acetone have obvious reduction.Illustrate under 120 DEG C of operating temperature, PPy/SnO2Nanometer tube composite materials for
NOx has high sensitivity and excellent selectivity.
Embodiment 2:0.8g PVP is added to stirring 2h in 9ml absolute ethyl alcohol and obtains solution A, by 1.2 g's
SnCl2•2H2O is added to stirring 2.5h in 5ml DMF and obtains solution B, then pours into solution A in B solution, and stir 2h and obtain
To transparent precursor solution.
Spinning is carried out using electrostatic spinning technique, it is 10kV to set direct current spinning voltage, the solidification of nozzle and receiver away from
From for 15cm, the PVP composite nano fibers containing presoma are obtained.PVP composite nano fibers are put into annealing furnace, in air atmosphere
Middle carry out calcination processing, from room temperature to 600 DEG C, programming rate is 15 DEG C/min, calcination time 3h, afterwards with body of heater from
Room temperature is so cooled to, obtains SnO2Nanotube fibers.
By 10mg lauryl sodium sulfate and 0.05g SnO2Hollow Nano fiber in use is added separately in the 50ml aqueous solution
3h is stirred at room temperature, adds 7.755 μ l Py monomers afterwards and stirs 1h, be eventually adding 3.3ml FeCl3The aqueous solution(Concentration is
0.1mol/L), liquid phase chemical oxidative polymerization is carried out in the case where being kept stirring for, is filtered and is cleaned after 5h, is obtained
PPy/SnO2Nanometer tube composite materials.
Air-sensitive performance test has been carried out in the gas sensor that 120 DEG C make gained composite, the results showed that with
SnO2Obtained PPy/SnO2Nanometer tube composite materials have high sensitivity and excellent selectivity for NOx.
Embodiment 3:0.7g PVP is added to stirring 2h in 8ml absolute ethyl alcohol and obtains solution A, by 0.6 g chlorination
Stannous(SnCl2•2H2O)It is added to stirring 2h in 3ml DMF and obtains solution B, then pours into solution A in B solution, and stir
2h obtains transparent precursor solution.
Spinning is carried out using electrostatic spinning technique, the solidification distance that direct current spinning voltage is 5kV, nozzle and receiver is set
For 13cm, the PVP composite nano fibers containing presoma are obtained.PVP composite nano fibers are put into annealing furnace, in air atmosphere
Carry out calcination processing, from room temperature to 550 DEG C, programming rate be 10 DEG C/min, calcination time 2.5h, afterwards with body of heater oneself
Room temperature is so cooled to, obtains SnO2Nanotube fibers.
By 10mg neopelex and 0.03g SnO2Hollow Nano fiber in use is added separately to the 50ml aqueous solution
In 1h is stirred at room temperature, add 2.585 μ l Py monomers afterwards and stir 1h, be eventually adding 1.1ml FeCl3The aqueous solution(Concentration
For 0.1mol/L), liquid phase chemical oxidative polymerization is carried out in the case where being kept stirring for, is filtered and is cleaned after 4h, obtained
Obtain PPy/SnO2Nanometer tube composite materials.
Embodiment 4:1.2g PVP is added to stirring 2h in 13ml absolute ethyl alcohol and obtains solution A, by 1.0 g chlorine
Change stannous be added to 7ml DMF stirring 2h obtain solution B, then solution A is poured into B solution, and stir 4h obtain it is transparent
Precursor solution.
Spinning is carried out using electrostatic spinning technique, it is 15kV to set direct current spinning voltage, the solidification of nozzle and receiver away from
From for 20cm, the PVP composite nano fibers containing presoma are obtained.PVP composite nano fibers are put into annealing furnace, in air atmosphere
Middle carry out calcination processing, from room temperature to 650 DEG C, programming rate is 13 DEG C/min, calcination time 6h, afterwards with body of heater from
Room temperature is so cooled to, obtains SnO2Nanotube fibers.
By 10mg lauryl sodium sulfate and 0.15g SnO2Hollow Nano fiber in use is added separately in the 50ml aqueous solution
3h is stirred at room temperature, adds 7.585 μ l Py monomers afterwards and stirs 1h, be eventually adding 3.2ml FeCl3The aqueous solution(Concentration is
0.1mol/L), liquid phase chemical oxidative polymerization is carried out in the case where being kept stirring for, is filtered and is cleaned after 5h, is obtained
PPy/SnO2Nanometer tube composite materials.
Embodiment 5:1.1g PVP is added to stirring 2h in 12ml absolute ethyl alcohol and obtains solution A, by 1.1 g chlorine
Change stannous be added in 8ml DMF stir 2h obtain solution B, then solution A is poured into B solution, and stir 2h obtain it is transparent
Precursor solution.
Spinning is carried out using electrostatic spinning technique, it is 16kV to set direct current spinning voltage, the solidification of nozzle and receiver away from
From for 25cm, the PVP composite nano fibers containing presoma are obtained.PVP composite nano fibers are put into annealing furnace, in air atmosphere
Middle carry out calcination processing, from room temperature to 700 DEG C, programming rate is 9 DEG C/min, calcination time 10h, afterwards with body of heater from
Room temperature is so cooled to, obtains SnO2Nanotube fibers.
By 18mg neopelex and 0.15g SnO2Hollow Nano fiber in use is added separately to the 50ml aqueous solution
In 3h is stirred at room temperature, add 7.755 μ l Py monomers afterwards and stir 1h, be eventually adding 3.3ml FeCl3The aqueous solution(Concentration
For 0.1mol/L), liquid phase chemical oxidative polymerization is carried out in the case where being kept stirring for, is filtered and is cleaned after 4h, obtained
Obtain PPy/SnO2Nanometer tube composite materials.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God any modification, equivalent substitution and improvements made etc., should be included in the scope of the protection with principle.
Claims (5)
- It is 1. a kind of to NOXPPy/SnO with high selectivity2Nanotube composite air-sensitive material, it is characterised in that be according to following sides Prepared by formula:(1)Configure SnO2The precursor solution of nanofiber:0.7-1.2g PVP is added in 8-13ml absolute ethyl alcohol and stirred Mix 1-3h and obtain solution A, by 0.6-1.2 g SnCl2•2H2O is added to stirring 1-2h in 3-8ml DMF and obtains solution B, so Solution A is poured into B solution afterwards, and stirs 2-4h and obtains transparent precursor solution;(2)Electrostatic spinning prepares PVP composite nano fibers:By step(1)In precursor solution be fitted into syringe, use is quiet Electrospinning carries out spinning and obtains PVP composite nano fibers;(3)Calcining prepares SnO2Nanotube fibers:By step(2)In PVP composite nano fibers be put into annealing furnace, in air Calcination processing is carried out in atmosphere, from room temperature to 550~700 DEG C, programming rate is not less than 10 DEG C/min, calcination time 1.5 ~10h, room temperature is naturally cooled to body of heater afterwards, obtain SnO2Nanotube fibers;(4)Prepare PPy/SnO2Nanometer tube composite materials:By 5-25mg surfactant and 0.03-0.2g SnO2Nanowire Dimension is added separately in the 50ml aqueous solution, and 1-3h is stirred at room temperature, and is added 1.5-8 μ l Py monomers afterwards and is stirred 0.5-2h, most The FeCl that concentration is 0.1mol/L is added afterwards3Aqueous solution 1-5ml, reacted under stirring, carry out filtering after 2-7h and clear Wash, obtain PPy/SnO2Nanometer tube composite materials.
- 2. as claimed in claim 1 to NOXPPy/SnO with high selectivity2Nanotube composite air-sensitive material, its feature exist In:Step(2)The condition of middle electrostatic spinning technique is:Direct current spinning voltage is 5~16 kV, the solidification of nozzle and receiver away from From for 10~25cm.
- 3. as claimed in claim 1 to NOXPPy/SnO with high selectivity2Nanotube composite air-sensitive material, its feature exist In:The surfactant is lauryl sodium sulfate or neopelex.
- 4. as described in one of claim 1 ~ 3 to NOXPPy/SnO with high selectivity2Nanotube composite air-sensitive material, its It is characterised by:Step(1)In be by 1g PVP be added in 10ml absolute ethyl alcohol stir 2h obtain solution A, by 0.8 g's SnCl2•2H2O be added to 4ml DMF stirring 2h obtain solution B, then solution A is poured into B solution, and stir 2h obtain it is transparent Precursor solution.
- 5. as described in one of claim 1 ~ 3 to NOXPPy/SnO with high selectivity2Nanotube composite air-sensitive material, its It is characterised by:Step(1)In be by 0.8g PVP be added in 9ml absolute ethyl alcohol stir 2h obtain solution A, by 1.2 g's SnCl2•2H2The DMF stirrings 2.5h that O is added to 5ml obtains solution B, and then solution A is poured into B solution, and is stirred 2h and obtained Bright precursor solution.
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