CN101266225A - Electric spinning method for preparing high performance ceramic base nanometer fibre gas-sensitive sensor - Google Patents
Electric spinning method for preparing high performance ceramic base nanometer fibre gas-sensitive sensor Download PDFInfo
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- CN101266225A CN101266225A CNA2008100506605A CN200810050660A CN101266225A CN 101266225 A CN101266225 A CN 101266225A CN A2008100506605 A CNA2008100506605 A CN A2008100506605A CN 200810050660 A CN200810050660 A CN 200810050660A CN 101266225 A CN101266225 A CN 101266225A
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Abstract
The invention provides a method for producing high performance ceramic semiconductor metal oxide nm fiber ethanol gas sensor using electric fiber spinning process. The soluble metal salt, metal oxide precursor, macromolecule and solvent are used as raw material and the complex fiber containing macromolecule and metal oxide precursor is prepared using the electric fiber spinning process and then the fiber is sintered to remove the macromolecule to obtain the ceramic semiconductor metal oxide nm fiber material. The unidimensional and continuous ceramic semiconductor metal oxide nm fiber ethanol gas sensor of king size has features: rapid answering and renewing, high sensitivity, good gas selectivity, good stability and long use life. The method is suitable for all kinds of ceramic oxide using the soluble metal salt as raw material with advantages of simple device, low cost, high performance and easy to popularize. The said method can satisfy the technology requirement and can be widely used in traffic safety, environment protection, chemical production and so on.
Description
Technical field
The invention belongs to ceramic base metal oxide semiconductor gas sensor technology of preparing, be specifically related to a kind of method of utilizing electrospinning silk technology to prepare high performance ceramic base metal oxide semiconductor nanometer fibre gas-sensitive sensor.
Background technology
Along with the develop rapidly of auto industry and road traffic cause, the traffic hazard incidence is in rising trend.Because the generation of traffic hazard not only causes a tremendous loss of lives, give countless families Jonah, and having a strong impact on economic development and social stability, caused the great attention and the concern of national governments.Studies show that in a large number: driving when intoxicated is one of main accident reason.Detect driver's the situation of drinking for convenience, rapidly, exactly, prevent the generation of such traffic hazard, press for function admirable, cheap, detect alcohol gas sensor rapidly.
Summary of the invention
The objective of the invention is: a kind of method of utilizing the electrospinning silk to prepare high performance ceramic base metal oxide semiconductor nanometer fibre gas-sensitive sensor is provided.
Electrospinning silk technology is that the high polymeric solution of non-Newtonian fluid overcomes surface tension and viscoelasticity power under high-voltage electric field, carries out the stretch bending campaign and obtains the technology of nanometer to Sub-micro Fibers.This technology has advantages such as equipment is simple, and production cost is low, and materials used is extensive and the output fiber size is even, and specific surface area is big.The present invention utilizes the overlength continuity of electricity spinning fibre just, and the excellent physical chemistry of the advantages metal oxide semiconductor that specific surface is big is prepared the continuous metal oxide semiconductor ceramic nanofibers gas sensor of one-dimensional super long.Ceramic base nanometer fibre gas-sensitive sensor by this method can be prepared in the response-recovery time, increases significantly on the performance index such as sensitivity, as, ZnO and SnO
2Sensitivity when the 100ppm is respectively the nanofiber gas sensor to the alcohol gas gas concentration: 10,20 all greater than 4; Response/release time is all less than 10 seconds.
Adopt the high performance ceramic base nanometer fibre alcohol gas gas sensor of this method preparation; not only the other technologies index is as having the advanced level that all reaches in response-recovery speed fast, highly sensitive, stable, serviceable life etc. in the international like product; can satisfy the requirement of industrial technology; can use widely in the fields such as environmental protection, Chemical Manufacture in traffic safety.
Electric spinning method for preparing high performance ceramic base semiconductor nano fibre air-sensitive sensor, it comprises the steps:
A. 0.5～5.0g water-soluble high-molecular compound is added in 10～20ml distilled water,, clarify fully to solution 100 ℃ of following reflux 4～6 hours; Behind cool to room temperature, the surfactant Qu Latong-x100 (Triton-x100) that adds 0.1～0.3ml in system stirred 1～3 hour, and it is mixed;
B. 0.1～2.0g soluble metallic salt is joined in 5～10ml distilled water, be stirred to dissolving; Then metal salt solution is joined in the solution of steps A, stir and after 1～3 hour solution is mixed;
C. the solution that step B is obtained is put into glass spray fiber tube, glass spray fiber tube head internal diameter is 0.5mm～3mm, with the aluminium cover is anode, accept product with aluminium foil as negative electrode, distance is 10～30cm between two-plate, apply 6～30KV voltage and carry out the electrospinning silk, after spinning in 12～72 hours, the nano fibrous membrane of the pbz polymer template that will obtain on cathode plate places vacuum drying oven, dried 6～8 hours down at 70 ℃, then 400～700 ℃ of following sintering 3～5 hours removing the macromolecule template, thereby obtain fibre diameter 50～300nm, have the ceramic base semiconductor nano fibre air-sensitive sensor of quick-speed response-recovery speed.
Water-soluble high-molecular compound described in the inventive method is polyvinyl alcohol (PVA) or polyvinylpyrrolidone; Described soluble metallic salt is a soluble zinc salt, as zinc acetate, zinc nitrate or zinc chloride; The solubility pink salt is as butter of tin or stannous chloride; Soluble ferric iron salt is as ferrous acetate, ferric nitrate or iron chloride.
All macromolecule raw materials described in the inventive method and surfactant all can obtain with commercial form from U.S. Aldrich chemical reagents corporation.All slaines and solvent all can obtain with commercial form from sky, Tianjin Thailand fine chemicals company limited.
Mechanism of the present invention can be done following understanding: the laggard horizontal high voltage blending of soluble metallic salt or oxide precursor and macromolecule mixed dissolution, obtaining with the macromolecule is the composition fiber of template.According to selected metal precursor and macromolecule, select suitable sintering temperature and heating schedule, at high temperature, make slaine oxidation at high temperature and crystallization simultaneously, form ceramic semiconductors metal oxide based nano-fiber the macromolecule template burn off in the composition fiber.The mechanism of the ceramic base metal oxide semiconductor alcohol gas gas sensor of the present invention's preparation is: belong to surface resistance control type mechanism.Concrete principle is: ZnO, SnO
2, Fe
2O
3Be N-type semiconductor, the oxygen in the easy absorbed air in its surface, its conduction band electron is transferred to make on oxygen molecule or the oxygen atom and is formed ionic link between them, promptly forms chemically adsorbing oxygen O
2Or O
-:
O
2(gas)＝O
2 -(ad)＝O
2(ad)＝O
-(ad)＝O
2-(ad)＝O
2-(lat)
(gas, ad, lat represent ambient oxygen respectively, adsorb oxygen and Lattice Oxygen) causes the material surface carrier concentration to descend owing to the absorption of oxygen, and surface conductance reduces, thereby component resistance is increased, even element also presents high resistance state in the air of cleaning; When element contact reducibility gas (as alcohol gas), surface adsorbed oxygen is easy to take place with it redox reaction, and the result has removed adsorb oxygen O
2Or O
-The electronics of absorption, these electronics return superficial layer to be caused surface barrier to reduce helping electronics moving to the border, reduces the order that reaches detection so surface conductance increases component resistance.
Preparing that the present invention is successful in the world first has response/recovery rapidly, highly sensitive ceramic base nanometer fibre gas-sensitive sensor, and it is simple to have preparation technology, be convenient to operation and advantage such as repeat, and production equipment is simple and convenient, and is lower to the working condition requirement, low production cost.The gained gas sensor not only has response-recovery speed fast, high sensitivity, and other every correlation technique indexs all meet or exceed international most advanced level, have wide market application prospect, are easy to promotion and application.
Description of drawings
Fig. 1: be electrospinning silk equipment work synoptic diagram used in the present invention;
Fig. 2: embodiment 1 prepared zinc oxide nano fiber stereoscan photograph;
Fig. 3: embodiment 1 prepared zinc oxide nano fiber transmission electron microscope photo;
Fig. 4: embodiment 10 prepared polyvinylpyrrolidones and tin chloride composition fiber scanning electron microscope sheet;
Fig. 5: embodiment 10 prepared tin oxide nano fiber stereoscan photographs;
Fig. 6: embodiment 13 prepared di-iron trioxide nanofiber stereoscan photographs;
Fig. 7: embodiment 13 prepared di-iron trioxide nanofiber transmission electron microscope photos;
Sensitivity-gas concentration the curve of the gas sensor that Fig. 8: embodiment 1 prepared zinc oxide nano fiber is made;
The response-recovery curve of the gas sensor that Fig. 9: embodiment 1 prepared zinc oxide nano fiber is made;
Figure 10: embodiment 10 prepared tin ash composition fiber sensitivity curves;
Figure 11: embodiment 10 prepared tin ash composition fiber response-recovery curves, the response-recovery curve map of single amplification;
The response-recovery curve of the gas sensor that Figure 12: embodiment 13 prepared di-iron trioxide nanofibers are made;
Sensitivity-gas concentration the curve of the gas sensor that Figure 13: embodiment 13 prepared di-iron trioxide nanofibers are made.
As shown in Figure 1,1 is high-voltage power supply, and 2 are glass spray fiber tube, 3 polymer/metal mixed salt solutions for ejecting, 4 be metal electrode as anode, 5 are the nanofiber of splitting, 6 is that the aluminium foil receiver sheet is as negative electrode.
As shown in Figure 2, embodiment 1 prepared zinc oxide nano fiber stereoscan photograph, the nanofiber fiber pattern of the zinc paste that makes of the present invention is good as can be seen, and diameter homogeneous, fibre diameter are distributed between 50～300 nanometers substantially.
As shown in Figure 3, embodiment 1 prepared zinc oxide nano fiber transmission electron microscope photo, the nanofiber surface of the zinc paste that makes of the present invention is coarse as can be seen, diameter homogeneous, fibre diameter are distributed between 50～260 nanometers substantially.
As shown in Figure 4, embodiment 10 prepared polyvinylpyrrolidones and tin chloride composition fiber stereoscan photograph, the composite nano fiber pattern that makes of the present invention is good as can be seen, and diameter homogeneous, fibre diameter are distributed between 50～280 nanometers substantially.
As shown in Figure 5, embodiment 10 prepared tin oxide nano fiber stereoscan photographs, the nanofiber pattern of the tin oxide that makes of the present invention is good as can be seen, and diameter homogeneous, fibre diameter are distributed between 50～280 nanometers substantially.
As shown in Figure 6, embodiment 13 prepared di-iron trioxide nanofiber stereoscan photographs, the nanofiber pattern of the di-iron trioxide that makes of the present invention is good as can be seen, and diameter homogeneous, fibre diameter are distributed between 80～300 nanometers substantially.
As shown in Figure 7, embodiment 1 prepared zinc oxide nano fiber transmission electron microscope photo, the nanofiber pattern of the zinc paste that makes of the present invention is good as can be seen, and diameter homogeneous, fibre diameter are distributed between 50～300 nanometers substantially.
As shown in Figure 8, the zinc oxide nano fiber gas sensor that the present invention makes is along with the dense increase sensitivity of alcohol gas gas increases, and sensitivity is very high, can detect low alcohol gas concentration (10ppm).The present invention of this proof has high sensitivity.
As shown in Figure 9, the zinc oxide nano fiber gas sensor that the present invention makes is to the response-recovery curve of alcohol gas, response of the present invention as can be seen, and release time is basically all within 10 seconds, proof the present invention has response-recovery speed rapidly, and this index has reached international most advanced level.
As shown in figure 10, the prepared tin ash fiber of the present invention sensitivity curve gas sensor is along with the dense increase sensitivity of alcohol gas increases, and when the concentration of alcohol gas was 5000ppm, sensitivity can reach 175.The present invention of this proof has high sensitivity.
As shown in figure 11, the prepared tin ash composition fiber of the present invention response-recovery curve, single amplification loud recovery curve figure, as can be seen from the figure, when alcohol gas concentration was 100ppm, the response time was 4 seconds, be 9 seconds release time.
As shown in figure 12, the nanometer fibre gas-sensitive sensor of the di-iron trioxide that the present invention makes is along with the dense increase sensitivity of gas increases, and sensitivity is very high, can detect lower alcohol gas concentration (100ppm).The present invention of this proof has higher sensitivity.
As shown in figure 13, the response-recovery curve of the di-iron trioxide nanometer fibre gas-sensitive sensor that the present invention makes, response of the present invention as can be seen, release time are basically all within 10 seconds.
Embodiment
1, utilize electrical spinning method to prepare the zinc oxide nano fiber gas sensor
Embodiment 1:
In the 50ml conical flask, the 1.0g polyvinyl alcohol (PVA) is added in the 15ml distilled water, 100 ℃ of following reflux 4 hours, clarify fully to solution.Behind the cool to room temperature, in solution, add 0.1ml Triton-x100 and continue to stir 1 hour to even.
Other gets a 50ml conical flask, adds the 0.75g zinc acetate successively, and 5ml distilled water stirs 10min to dissolving fully under the room temperature.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour.
The solution that mixes is put into the spray fiber tube, and the internal diameter of spinning head is 1mm, as anode, accepts product with aluminium foil as negative electrode with the aluminium cover, and two die openings are from being 20cm, and applying voltage is that 15kV carries out the electrospinning silk.After spinning in 40 hours, the nano fibrous membrane that receives on the minus plate is dried 6 hours except that desolvating under 70 ℃ in vacuum drying oven, put into muffle furnace then, slowly be warming up to 600 ℃ of constant temperature sintering 5 hours.Gained zinc oxide nano fiber diameter is about 130～250nm, thus obtained zinc oxide nano fiber gas sensor is 300 degrees centigrade in working temperature, sensitivity was 76 when the concentration of alcohol gas was 5000ppm, when the concentration of alcohol gas is 1000ppm, response time is 3 seconds, and be 10 seconds release time.
Embodiment 2:
In the 50ml conical flask, the 1.0g polyvinylpyrrolidone is added in the 15ml distilled water, 100 ℃ of following reflux 4 hours, clarify fully to solution.Behind the cool to room temperature, in solution, add 0.1mlTriton-x100 and continue to stir 1 hour to even.Other gets a 50ml conical flask, adds the 1.0g zinc acetate successively, and 5ml distilled water stirs 10min to dissolving fully under the room temperature.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour.The solution that mixes is put into the spray fiber tube, and the internal diameter of spinning head is 1mm, as anode, accepts product with aluminium foil as negative electrode with the aluminium cover, and two die openings are from being 20cm, and applying voltage is that 15kV carries out the electrospinning silk.After spinning in 40 hours, the nano fibrous membrane that receives on the minus plate is dried 6 hours except that desolvating under 70 ℃ in vacuum drying oven, put into muffle furnace then, slowly be warming up to 600 ℃ of constant temperature sintering 5 hours.Gained zinc oxide nano fiber diameter is about 150～280nm, thus obtained zinc oxide nano fiber gas sensor is 300 degrees centigrade in working temperature, sensitivity was 75 when the concentration of alcohol gas was 5000ppm, when the concentration of alcohol gas is 1000ppm, response time is 2 seconds, and be 9 seconds release time.
Embodiment 3:
In the 50ml conical flask, the 1.0g polyvinyl alcohol (PVA) is added in the 15ml distilled water, 100 ℃ of following reflux 4 hours, clarify fully to solution.Behind the cool to room temperature, in solution, add 0.1ml Triton-x100 and continue to stir 1 hour to even.Other gets a 50ml conical flask, adds the 1.25g zinc acetate successively, and 5ml distilled water stirs 10min to dissolving fully under the room temperature.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour.The solution that mixes is put into the spray fiber tube, and the internal diameter of spinning head is 1mm, as anode, accepts product with aluminium foil as negative electrode with the aluminium cover, and two die openings are from being 20cm, and applying voltage is that 15kV carries out the electrospinning silk.After spinning in 40 hours, the nano fibrous membrane that receives on the minus plate is dried 6 hours except that desolvating under 70 ℃ in vacuum drying oven, put into muffle furnace then, slowly be warming up to 600 ℃ of constant temperature sintering 5 hours.Gained zinc oxide nano fiber diameter is about 150～250nm, thus obtained zinc oxide nano fiber gas sensor is 300 degrees centigrade in working temperature, sensitivity was 72 when the concentration of alcohol gas was 5000ppm, when the concentration of alcohol gas is 1000ppm, response time is 5 seconds, and be 10 seconds release time.
Embodiment 4:
In the 50ml conical flask, the 1.0g polyvinyl alcohol (PVA) is added in the 15ml distilled water, 100 ℃ of following reflux 4 hours, clarify fully to solution.Behind the cool to room temperature, in solution, add 0.1ml triton-x100 and continue to stir 1 hour to even.Other gets a 50ml conical flask, adds the 0.75g zinc nitrate successively, and 5ml distilled water stirs 10min to dissolving fully under the room temperature.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour.The solution that mixes is put into the spray fiber tube, and the internal diameter of spinning head is 1mm, as anode, accepts product with aluminium foil as negative electrode with the aluminium cover, and two die openings are from being 20cm, and applying voltage is that 15kV carries out the electrospinning silk.After spinning in 40 hours, the nano fibrous membrane that receives on the minus plate is dried 6 hours except that desolvating under 70 ℃ in vacuum drying oven, put into muffle furnace then, slowly be warming up to 600 ℃ of constant temperature sintering 5 hours.Gained zinc oxide nano fiber diameter is about 150～300nm, thus obtained zinc oxide nano fiber gas sensor is 300 degrees centigrade in working temperature, sensitivity was 71 when the concentration of alcohol gas was 5000ppm, when the concentration of alcohol gas is 1000ppm, response time is 4 seconds, and be 10 seconds release time.
Embodiment 5:
In the 50ml conical flask, the 1.0g polyvinyl alcohol (PVA) is added in the 15ml distilled water, 100 ℃ of following reflux 4 hours, clarify fully to solution.Behind the cool to room temperature, in solution, add 0.1ml triton-x100 and continue to stir 1 hour to even.Other gets a 50ml conical flask, adds the 1.0g zinc nitrate successively, and 5ml distilled water stirs 10min to dissolving fully under the room temperature.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour.The solution that mixes is put into the spray fiber tube, and the internal diameter of spinning head is 1mm, as anode, accepts product with aluminium foil as negative electrode with the aluminium cover, and two die openings are from being 20cm, and applying voltage is that 15kV carries out the electrospinning silk.After spinning in 40 hours, the nano fibrous membrane that receives on the minus plate is dried 6 hours except that desolvating under 70 ℃ in vacuum drying oven, put into muffle furnace then, slowly be warming up to 600 ℃ of constant temperature sintering 5 hours.Gained zinc oxide nano fiber diameter is about 150～250nm, thus obtained zinc oxide nano fiber gas sensor is 300 degrees centigrade in working temperature, sensitivity was 73 when the concentration of alcohol gas was 5000ppm, when the concentration of alcohol gas is 1000ppm, response time is 3 seconds, and be 10 seconds release time.
Embodiment 6:
In the 50ml conical flask, the 1.0g polyvinyl alcohol (PVA) is added in the 15ml distilled water, 100 ℃ of following reflux 4 hours, clarify fully to solution.Behind the cool to room temperature, in solution, add 0.1ml triton-x100 and continue to stir 1 hour to even.Other gets a 50ml conical flask, adds the 1.25g zinc nitrate successively, and 5ml distilled water stirs 10min to dissolving fully under the room temperature.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour.The solution that mixes is put into the spray fiber tube, and the internal diameter of spinning head is 1mm, as anode, accepts product with aluminium foil as negative electrode with the aluminium cover, and two die openings are from being 20cm, and applying voltage is that 15kV carries out the electrospinning silk.After spinning in 40 hours, the nano fibrous membrane that receives on the minus plate is dried 6 hours except that desolvating under 70 ℃ in vacuum drying oven, put into muffle furnace then, slowly be warming up to 600 ℃ of constant temperature sintering 5 hours.Gained zinc oxide nano fiber diameter is about 130～200nm, thus obtained zinc oxide nano fiber gas sensor is 300 degrees centigrade in working temperature, sensitivity was 72 when the concentration of alcohol gas was 5000ppm, when the concentration of alcohol gas is 1000ppm, response time is 3 seconds, and be 10 seconds release time.
Embodiment 7:
In the 50ml conical flask, the 1.0g polyvinyl alcohol (PVA) is added in the 15ml distilled water, 100 ℃ of following reflux 4 hours, clarify fully to solution.Behind the cool to room temperature, in solution, add 0.1ml triton-x100 and continue to stir 1 hour to even.Other gets a 50ml conical flask, adds the 0.75g zinc chloride successively, and 5ml distilled water stirs 10min to dissolving fully under the room temperature.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour.The solution that mixes is put into the spray fiber tube, and the internal diameter of spinning head is 1mm, as anode, accepts product with aluminium foil as negative electrode with the aluminium cover, and two die openings are from being 20cm, and applying voltage is that 15kV carries out the electrospinning silk.After spinning in 40 hours, the nano fibrous membrane that receives on the minus plate is dried 6 hours except that desolvating under 70 ℃ in vacuum drying oven, put into muffle furnace then, slowly be warming up to 600 ℃ of constant temperature sintering 5 hours.Gained zinc oxide nano fiber diameter is about 120～180nm, thus obtained zinc oxide nano fiber gas sensor is 300 degrees centigrade in working temperature, sensitivity was 71 when the concentration of alcohol gas was 5000ppm, when the concentration of alcohol gas is 1000ppm, response time is 6 seconds, and be 9 seconds release time.
Embodiment 8:
In the 50ml conical flask, the 1.0g polyvinylpyrrolidone is added in the 15ml distilled water, 100 ℃ of following reflux 4 hours, clarify fully to solution.Behind the cool to room temperature, in solution, add 0.1mltriton-x100 and continue to stir 1 hour to even.Other gets a 50ml conical flask, adds the 1.0g zinc chloride successively, and 5ml distilled water stirs 10min to dissolving fully under the room temperature.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour.The solution that mixes is put into the spray fiber tube, and the internal diameter of spinning head is 1mm, as anode, accepts product with aluminium foil as negative electrode with the aluminium cover, and two die openings are from being 20cm, and applying voltage is that 15kV carries out the electrospinning silk.After spinning in 40 hours, the nano fibrous membrane that receives on the minus plate is dried 6 hours except that desolvating under 70 ℃ in vacuum drying oven, put into muffle furnace then, slowly be warming up to 600 ℃ of constant temperature sintering 5 hours.Gained zinc oxide nano fiber diameter is about 100～150nm, and thus obtained zinc oxide nano fiber gas sensor is 300 degrees centigrade in working temperature, and sensitivity was 70 when the concentration of alcohol gas was 5000ppm, and the response time is 4 seconds, and be 10 seconds release time.
Embodiment 9:
In the 50ml conical flask, the 1.0g polyvinyl alcohol (PVA) is added in the 15ml distilled water, 100 ℃ of following reflux 4 hours, clarify fully to solution.Behind the cool to room temperature, in solution, add 0.1ml triton-x100 and continue to stir 1 hour to even.Other gets a 50ml conical flask, adds the 1.25g zinc chloride successively, and 5ml distilled water stirs 10min to dissolving fully under the room temperature.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour.The solution that mixes is put into the spray fiber tube, and the internal diameter of spinning head is 1mm, as anode, accepts product with aluminium foil as negative electrode with the aluminium cover, and two die openings are from being 20cm, and applying voltage is that 15kV carries out the electrospinning silk.After spinning in 40 hours, the nano fibrous membrane that receives on the minus plate is dried 6 hours except that desolvating under 70 ℃ in vacuum drying oven, put into muffle furnace then, slowly be warming up to 600 ℃ of constant temperature sintering 5 hours.Gained zinc oxide nano fiber diameter is about 130～180nm, thus obtained zinc oxide nano fiber gas sensor is 300 degrees centigrade in working temperature, sensitivity was 74 when the concentration of alcohol gas was 5000ppm, when the concentration of alcohol gas is 1000ppm, response time is 3 seconds, and be 9 seconds release time.
2, utilize electrical spinning method to prepare the tin dioxide nano fiber gas sensor
Embodiment 10:
In the 50ml conical flask, the 1.0g polyvinylpyrrolidone is added in the 15ml distilled water, 100 ℃ of following reflux 4 hours, clarify fully to solution.Behind the cool to room temperature, in solution, add 0.1mltriton-x100 and continue to stir 1 hour to even.
Other gets a 50ml conical flask, adds the 0.5g butter of tin successively, and 5ml distilled water stirs 10min to dissolving fully under the room temperature.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour.
The solution that mixes is put into the spray fiber tube, and the internal diameter of spinning head is 1mm, as anode, accepts product with aluminium foil as negative electrode with the aluminium cover, and two die openings are from being 20cm, and applying voltage is that 15kV carries out the electrospinning silk.After spinning in 50 hours, the nano fibrous membrane that receives on the minus plate is dried 6 hours except that desolvating under 70 ℃ in vacuum drying oven, put into muffle furnace then, slowly be warming up to 600 ℃ of constant temperature sintering 5 hours.Gained zinc oxide nano fiber diameter is about 130～180nm, thus obtained tin oxide nano fibre air-sensitive element is 300 degrees centigrade in working temperature, sensitivity was 174 when the concentration of alcohol gas was 5000ppm, the concentration of alcohol gas is 3 seconds for the 100ppm response time, and be 9 seconds release time.
Embodiment 11:
In the 50ml conical flask, the 1.0g polyvinyl alcohol (PVA) is added in the 15ml distilled water, 100 ℃ of following reflux 4 hours, clarify fully to solution.Behind the cool to room temperature, in solution, add 0.1ml triton-x100 and continue to stir 1 hour to even.Other gets a 50ml conical flask, adds successively.0.75g stannous chloride, 5ml distilled water stirs 10min to dissolving fully under the room temperature.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour.The solution that mixes is put into the spray fiber tube, and the internal diameter of spinning head is 1mm, as anode, accepts product with aluminium foil as negative electrode with the aluminium cover, and two die openings are from being 20cm, and applying voltage is that 15kV carries out the electrospinning silk.After spinning in 50 hours, the nano fibrous membrane that receives on the minus plate is dried 6 hours except that desolvating under 70 ℃ in vacuum drying oven, put into muffle furnace then, slowly be warming up to 600 ℃ of constant temperature sintering 5 hours.Gained tin oxide nano fibre diameter is about 130～180nm, thus obtained tin oxide nano fibre air-sensitive element is 300 degrees centigrade in working temperature, sensitivity was 175 when the concentration of alcohol gas was 5000ppm, the concentration of alcohol gas is 4 seconds for the 100ppm response time, and be 9 seconds release time.
Embodiment 12:
In the 50ml conical flask, the 1.0g polyvinyl alcohol (PVA) is added in the 15ml distilled water, 100 ℃ of following reflux 4 hours, clarify fully to solution.Behind the cool to room temperature, in solution, add 0.1ml triton-x100 and continue to stir 1 hour to even.Other gets a 50ml conical flask, adds successively.1.25g butter of tin, 5ml distilled water stirs 10min to dissolving fully under the room temperature.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour.The solution that mixes is put into the spray fiber tube, and the internal diameter of spinning head is 1mm, as anode, accepts product with aluminium foil as negative electrode with the aluminium cover, and two die openings are from being 20cm, and applying voltage is that 15kV carries out the electrospinning silk.After spinning in 50 hours, the nano fibrous membrane that receives on the minus plate is dried 6 hours except that desolvating under 70 ℃ in vacuum drying oven, put into muffle furnace then, slowly be warming up to 600 ℃ of constant temperature sintering 5 hours.Gained tin oxide nano fibre diameter is about 130～180nm, thus obtained tin oxide nano fibre air-sensitive element is 300 degrees centigrade in working temperature, sensitivity was 174 when the concentration of alcohol gas was 5000ppm, the concentration of alcohol gas is to be 4s the 100ppm air-sensitive response time, and be 8s release time.
3. utilize electrical spinning method to prepare the di-iron trioxide nanometer fibre gas-sensitive sensor
Embodiment 13:
In the 50ml conical flask, the 1.0g polyvinyl alcohol (PVA) is added in the 15ml distilled water, 100 ℃ of following reflux 4 hours, clarify fully to solution.Behind the cool to room temperature, in solution, add 0.1ml triton-x100 and continue to stir 1 hour to even.
Other gets a 50ml conical flask, adds the 0.5g ferric nitrate successively, and 5ml distilled water stirs 10min to dissolving fully under the room temperature.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour.
The solution that mixes is put into the spray fiber tube, and the internal diameter of spinning head is 1mm, as anode, accepts product with aluminium foil as negative electrode with the aluminium cover, and two die openings are from being 20cm, and applying voltage is that 15kV carries out the electrospinning silk.After spinning in 48 hours, the nano fibrous membrane that receives on the minus plate is dried 6 hours except that desolvating under 70 ℃ in vacuum drying oven, put into muffle furnace then, slowly be warming up to 600 ℃ of constant temperature sintering 6 hours.Gained di-iron trioxide composite nano fiber diameter is about 180～250nm, obtaining di-iron trioxide nanometer fibre gas-sensitive element thus is 250 degrees centigrade in working temperature, sensitivity was 7 when the concentration of alcohol gas was 5000ppm, and the response time is 2 seconds, and be 9 seconds release time.
Embodiment 14:
In the 50ml conical flask, the 1.0g polyvinylpyrrolidone is added in the 15ml distilled water, 100 ℃ of following reflux 4 hours, clarify fully to solution.Behind the cool to room temperature, in solution, add 0.1mltriton-x100 and continue to stir 1 hour to even.Other gets a 50ml conical flask, adds the 1.0g ferric nitrate successively, and 5ml distilled water stirs 10min to dissolving fully under the room temperature.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour.The solution that mixes is put into the spray fiber tube, and the internal diameter of spinning head is 1mm, as anode, accepts product with aluminium foil as negative electrode with the aluminium cover, and two die openings are from being 20cm, and applying voltage is that 15kV carries out the electrospinning silk.After spinning in 48 hours, the nano fibrous membrane that receives on the minus plate is dried 6 hours except that desolvating under 70 ℃ in vacuum drying oven, put into muffle furnace then, slowly be warming up to 600 ℃ of constant temperature sintering 6 hours.Gained di-iron trioxide composite nano fiber diameter is about 180～300nm, obtaining di-iron trioxide nanometer fibre gas-sensitive element thus is 250 degrees centigrade in working temperature, sensitivity was 6.8 when the concentration of alcohol gas was 5000ppm, and the response time is 3 seconds, and be 8 seconds release time.
Embodiment 15:
In the 50ml conical flask, the 1.0g polyvinyl alcohol (PVA) is added in the 15ml distilled water, 100 ℃ of following reflux 4 hours, clarify fully to solution.Behind the cool to room temperature, in solution, add 0.1ml triton-x100 and continue to stir 1 hour to even.Other gets a 50ml conical flask, adds the 1.25g ferric nitrate successively, and 5ml distilled water stirs 10min to dissolving fully under the room temperature.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour.The solution that mixes is put into the spray fiber tube, and the internal diameter of spinning head is 1mm, as anode, accepts product with aluminium foil as negative electrode with the aluminium cover, and two die openings are from being 20cm, and applying voltage is that 15kV carries out the electrospinning silk.After spinning in 48 hours, the nano fibrous membrane that receives on the minus plate is dried 6 hours except that desolvating under 70 ℃ in vacuum drying oven, put into muffle furnace then, slowly be warming up to 600 ℃ of constant temperature sintering 6 hours.Gained di-iron trioxide composite nano fiber diameter is about 150～280nm, obtaining di-iron trioxide nanometer fibre gas-sensitive element thus is 250 degrees centigrade in working temperature, sensitivity was 6.7 when the concentration of alcohol gas was 5000ppm, and the response time is 4 seconds, and be 8 seconds release time.
Embodiment 16:
In the 50ml conical flask, the 1.0g polyvinyl alcohol (PVA) is added in the 15ml distilled water, 100 ℃ of following reflux 4 hours, clarify fully to solution.Behind the cool to room temperature, in solution, add 0.1ml triton-x100 and continue to stir 1 hour to even.Other gets a 50ml conical flask, adds the 0.5g ferrous acetate successively, and 5ml distilled water stirs 10min to dissolving fully under the room temperature.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour.The solution that mixes is put into the spray fiber tube, and the internal diameter of spinning head is 1mm, as anode, accepts product with aluminium foil as negative electrode with the aluminium cover, and two die openings are from being 20cm, and applying voltage is that 15kV carries out the electrospinning silk.After spinning in 48 hours, the nano fibrous membrane that receives on the minus plate is dried 6 hours except that desolvating under 70 ℃ in vacuum drying oven, put into muffle furnace then, slowly be warming up to 600 ℃ of constant temperature sintering 6 hours.Gained di-iron trioxide composite nano fiber diameter is about 120～200nm, obtaining di-iron trioxide nanometer fibre gas-sensitive element thus is 250 degrees centigrade in working temperature, sensitivity was 7 when the concentration of alcohol gas was 5000ppm, and the response time is 3 seconds, and be 7 seconds release time.
Embodiment 17:
In the 50ml conical flask, the 1.0g polyvinylpyrrolidone is added in the 15ml distilled water, 100 ℃ of following reflux 4 hours, clarify fully to solution.Behind the cool to room temperature, in solution, add 0.1mltriton-x100 and continue to stir 1 hour to even.Other gets a 50ml conical flask, adds the 1.0g ferrous acetate successively, and 5ml distilled water stirs 10min to dissolving fully under the room temperature.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour.The solution that mixes is put into the spray fiber tube, and the internal diameter of spinning head is 1mm, as anode, accepts product with aluminium foil as negative electrode with the aluminium cover, and two die openings are from being 20cm, and applying voltage is that 15kV carries out the electrospinning silk.After spinning in 48 hours, the nano fibrous membrane that receives on the minus plate is dried 6 hours except that desolvating under 70 ℃ in vacuum drying oven, put into muffle furnace then, slowly be warming up to 600 ℃ of constant temperature sintering 6 hours.Gained di-iron trioxide composite nano fiber diameter is about 150～280nm, obtaining di-iron trioxide nanometer fibre gas-sensitive element thus is 250 degrees centigrade in working temperature, sensitivity was 7 when the concentration of alcohol gas was 5000ppm, and the response time is 5 seconds, and be 10 seconds release time.
Embodiment 18:
In the 50ml conical flask, the 1.0g polyvinyl alcohol (PVA) is added in the 15ml distilled water, 100 ℃ of following reflux 4 hours, clarify fully to solution.Behind the cool to room temperature, in solution, add 0.1ml triton-x100 and continue to stir 1 hour to even.Other gets a 50ml conical flask, adds the 1.5g ferrous acetate successively, and 5ml distilled water stirs 10min to dissolving fully under the room temperature.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour.The solution that mixes is put into the spray fiber tube, and the internal diameter of spinning head is 1mm, as anode, accepts product with aluminium foil as negative electrode with the aluminium cover, and two die openings are from being 20cm, and applying voltage is that 15kV carries out the electrospinning silk.After spinning in 48 hours, the nano fibrous membrane that receives on the minus plate is dried 6 hours except that desolvating under 70 ℃ in vacuum drying oven, put into muffle furnace then, slowly be warming up to 600 ℃ of constant temperature sintering 6 hours.Gained di-iron trioxide composite nano fiber diameter is about 130～230nm, obtaining di-iron trioxide nanometer fibre gas-sensitive element thus is 250 degrees centigrade in working temperature, sensitivity was 6.5 when the concentration of alcohol gas was 5000ppm, and the response time is 4 seconds, and be 9 seconds release time.
Embodiment 19:
In the 50ml conical flask, the 1.2g polyvinyl alcohol (PVA) is added in the 15ml distilled water, 100 ℃ of following reflux 4 hours, clarify fully to solution.Behind the cool to room temperature, in solution, add 0.1ml triton-x100 and continue to stir 1 hour to even.Other gets a 50ml conical flask, adds 0.5g iron chloride, 5ml distilled water successively, stirs 10min under the room temperature to dissolving fully.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour.The solution that mixes is put into the spray fiber tube, and the internal diameter of spinning head is 1mm, as anode, accepts product with aluminium foil as negative electrode with the aluminium cover, and two die openings are from being 20cm, and applying voltage is that 15kV carries out the electrospinning silk.After spinning in 48 hours, the nano fibrous membrane that receives on the minus plate is dried 6 hours except that desolvating under 70 ℃ in vacuum drying oven, put into muffle furnace then, slowly be warming up to 600 ℃ of constant temperature sintering 6 hours.Gained di-iron trioxide composite nano fiber diameter is about 150～180nm, obtaining di-iron trioxide nanometer fibre gas-sensitive element thus is 250 degrees centigrade in working temperature, sensitivity was 5.9 when the concentration of alcohol gas was 5000ppm, and the response time is 5 seconds, and be 9 seconds release time.
Embodiment 20:
In the 50ml conical flask, the 1.0g polyvinyl alcohol (PVA) is added in the 15ml distilled water, 100 ℃ of following reflux 4 hours, clarify fully to solution.Behind the cool to room temperature, in solution, add 0.1ml triton-x100 and continue to stir 1 hour to even.Other gets a 50ml conical flask, adds 1g iron chloride successively, and 5ml distilled water stirs 10min to dissolving fully under the room temperature.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour.The solution that mixes is put into the spray fiber tube, and the internal diameter of spinning head is 1mm, as anode, accepts product with aluminium foil as negative electrode with the aluminium cover, and two die openings are from being 20cm, and applying voltage is that 15kV carries out the electrospinning silk.After spinning in 48 hours, the nano fibrous membrane that receives on the minus plate is dried 6 hours except that desolvating under 70 ℃ in vacuum drying oven, put into muffle furnace then, slowly be warming up to 600 ℃ of constant temperature sintering 6 hours.Gained di-iron trioxide composite nano fiber diameter is about 180～250nm, obtaining di-iron trioxide nanometer fibre gas-sensitive element thus is 250 degrees centigrade in working temperature, sensitivity was 6.8 when the concentration of alcohol gas was 5000ppm, and the response time is 4 seconds, and be 10 seconds release time.
Embodiment 21:
In the 50ml conical flask, the 1.0g polyvinylpyrrolidone is added in the 15ml distilled water, 100 ℃ of following reflux 4 hours, clarify fully to solution.Behind the cool to room temperature, in solution, add 0.1mltriton-x100 and continue to stir 1 hour to even.Other gets a 50ml conical flask, adds 1.5g iron chloride successively, and 5ml distilled water stirs 10min to dissolving fully under the room temperature.Polymer Solution is mixed with metal salt solution, continue at room temperature to stir 1 hour.The solution that mixes is put into the spray fiber tube, and the internal diameter of spinning head is 1mm, as anode, accepts product with aluminium foil as negative electrode with the aluminium cover, and two die openings are from being 20cm, and applying voltage is that 15kV carries out the electrospinning silk.After spinning in 48 hours, the nano fibrous membrane that receives on the minus plate is dried 6 hours except that desolvating under 70 ℃ in vacuum drying oven, put into muffle furnace then, slowly be warming up to 600 ℃ of constant temperature sintering 6 hours.Gained di-iron trioxide composite nano fiber diameter is about 140～290nm, obtaining di-iron trioxide nanometer fibre gas-sensitive element thus is 250 degrees centigrade in working temperature, sensitivity was 6.3 when the concentration of alcohol gas was 5000ppm, and the response time is 4 seconds, and be 10 seconds release time.
Claims (7)
1, electric spinning method for preparing high performance ceramic base semiconductor nano fibre air-sensitive sensor, it comprises the steps:
A. 0.5～5.0g water-soluble high-molecular compound is added in 10～20ml distilled water,, clarify fully to solution 100 ℃ of following reflux 4～6 hours; Behind cool to room temperature, the surfactant that adds 0.1～0.3ml in system stirred 1～3 hour, and it is mixed;
B. 0.1～2.0g soluble metallic salt is joined in 5～10ml distilled water, be stirred to dissolving; Then metal salt solution is joined in the solution of steps A, stir and after 1～3 hour solution is mixed;
C. the solution that step B is obtained is put into glass spray fiber tube, glass spray fiber tube head internal diameter is 0.5mm～3mm, with the aluminium cover is anode, accept product with aluminium foil as negative electrode, distance is 10～30cm between two-plate, apply 6～30KV voltage and carry out the electrospinning silk, after spinning in 12～72 hours, the nano fibrous membrane of the pbz polymer template that will obtain on cathode plate places vacuum drying oven, dried 6～8 hours down at 70 ℃, then 400～700 ℃ of following sintering 3～5 hours removing the macromolecule template, thereby obtain fibre diameter 50～300nm, have the ceramic base semiconductor nano fibre air-sensitive sensor of quick-speed response-recovery speed.
2, electric spinning method for preparing high performance ceramic base semiconductor nano fibre air-sensitive sensor as claimed in claim 1, it is characterized in that: water-soluble high-molecular compound is polyvinyl alcohol (PVA) or polyvinylpyrrolidone.
3, electric spinning method for preparing high performance ceramic base semiconductor nano fibre air-sensitive sensor as claimed in claim 1, it is characterized in that: soluble metallic salt is soluble zinc salt, solubility pink salt or soluble ferric iron salt.
4, electric spinning method for preparing high performance ceramic base semiconductor nano fibre air-sensitive sensor as claimed in claim 3, it is characterized in that: soluble zinc salt is butter of tin or stannous chloride.
5, electric spinning method for preparing high performance ceramic base semiconductor nano fibre air-sensitive sensor as claimed in claim 3, it is characterized in that: the solubility pink salt is butter of tin or stannous chloride.
6, electric spinning method for preparing high performance ceramic base semiconductor nano fibre air-sensitive sensor as claimed in claim 3, it is characterized in that: soluble ferric iron salt is ferrous acetate, ferric nitrate or iron chloride.
7, electric spinning method for preparing high performance ceramic base semiconductor nano fibre air-sensitive sensor as claimed in claim 1, it is characterized in that: surfactant is Qu Latong-x100.
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