CN102331443A - Acetone gas sensor and manufacturing method thereof - Google Patents
Acetone gas sensor and manufacturing method thereof Download PDFInfo
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- CN102331443A CN102331443A CN201110195804A CN201110195804A CN102331443A CN 102331443 A CN102331443 A CN 102331443A CN 201110195804 A CN201110195804 A CN 201110195804A CN 201110195804 A CN201110195804 A CN 201110195804A CN 102331443 A CN102331443 A CN 102331443A
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Abstract
The invention provides an acetone gas sensor and a manufacturing method thereof. The acetone gas sensor is characterized in that zinc oxide hollow nanometer fiber is used as a gas sensitive material, and the manufacturing method of the zinc oxide hollow nanometer fiber comprises the steps of carrying out homotaxial electrostatic spinning to a spinning solution containing zinc salt and high polymers, drying and then sintering to remove the high polymers. The invention has the advantages that the working temperature of the acetone gas sensor is reduced, the sensitivity of the acetone gas sensor is improved, and the acetone gas sensor has obvious response to low-concentration acetone gas and good selectivity to the acetone gas.
Description
Technical field
The present invention relates to a kind of acetone gas sensor and preparation method thereof.
Background technology
Zinc paste is a kind of typical n type, semiconductor material, has been used as a kind of high-performance gas sensitive at present and has been widely used in NO
2, H
2S, NH
3High-sensitivity detection etc. various toxic and harmfuls.Since S.Iijima found CNT in 1991, the research of one dimension hollow material just more and more caused people's great attention.Compare with common one-dimension zinc oxide material (nano wire, nano belt); The rock-steady structure that hollow zinc oxide nano fiber has higher specific surface area, more gas passage and is difficult for reuniting as gas sensitive, therefore significant for the gas sensor of developing high sensitivity, high selectivity, cost is low, energy consumption is little, stability is high.
Electrostatic spinning technique is that the high polymeric solution of non-Newtonian fluid overcomes existing tension force in surface 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 that equipment is simple, and production cost is low, and materials used extensively reaches advantages such as specific surface area is big.At present, the existing both at home and abroad report that utilizes the coaxial electrostatic spinning equipment to prepare the hollow metal oxide, but the coaxial electrostatic spinning equipment is comparatively complicated, and all there is difficulty in the setting of choice of Solvent and spinning parameter.Single shaft static spins and has then overcome above deficiency.
At present mainly concentrate on ZnO, SnO as the sensitive material research of acetone steam with oxide
2, CeO
2, material such as NiO; Wherein the sensitivity to the acetone gas of 100ppm when working temperature is 300 ℃ of the ZnO of dumb-bell shape and zinc oxide nano rod is respectively 26.1 and 30.4; Zinc-oxide film sensitivity to 100ppm acetone when working temperature is 400 ℃ is about 30; The working temperature of these materials is higher, and energy consumption is bigger; Through Eu
2O
3SnO after the modification
2Film sensitivity to the acetone gas of 1000ppm under 185 ℃ of working temperatures is more than 8; But owing to methyl alcohol, ethanol etc. can't carry out selective response with the acetone similar performance; And the LDL to acetone is also higher, and these problems have all been brought difficulty to practical application.
Summary of the invention
The purpose of this invention is to provide a kind of acetone gas sensor and preparation method thereof, the detection sensitivity to acetone is high under low working temperature, selectivity is good, stability is high for described acetone gas sensor.
In order to achieve the above object; The invention provides a kind of acetone gas sensor; It is characterized in that adopt the zinc oxide hollow nanofiber as gas sensitive, the preparation method of described zinc oxide hollow nanofiber comprises: the spinning solution that will contain zinc salt and high molecular polymer carries out the single shaft electrostatic spinning; Oven dry, the knot that reburns is removed macromolecule wherein.
Preferably; The described compound method that contains the spinning solution of zinc salt and high molecular polymer is: with water-soluble high-molecular compound with ethanol and N; The mixed solvent dissolving of dinethylformamide (DMF) obtains settled solution; Soluble zinc salt is obtained zinc solution with deionized water dissolving, the zinc solution of gained is dropwise joined in the above-mentioned settled solution, mix.
Described water soluble polymer is preferably polyvinylpyrrolidone (PVP).The mass ratio of ethanol and DMF is preferably 1:0.1～10 in the mixed solvent of described ethanol and DMF.The w/v of described water soluble polymer and mixed solvent is preferably 1g:5～10ml.
Described soluble zinc salt is preferably zinc acetate.The w/v of described soluble zinc salt and deionized water is preferably 1g:1～2.5ml.
The volume ratio of described zinc solution and settled solution is preferably 2:3～10.
Preferably; The actual conditions of described single shaft electrostatic spinning is: the spinning solution that will contain zinc salt and high molecular polymer joins in the liquid storage pipe of single shaft electrostatic spinning apparatus; With the spray silk syringe needle of liquid storage pipe as anode; As negative electrode, the distance between anode and the negative electrode is 10～30cm with the aluminium foil dash receiver, and the voltage that applies 10～30V carries out the single shaft electrostatic spinning.
More preferably, the air themperature of described single shaft electrostatic spinning is 45～60%, and the spinning time is 10～14 hours.
Preferably, the temperature of described oven dry is that 80～100 ℃, time are 3～5 hours.
Preferably, described sintering temperature is 500～700 ℃, and the time is 1～5 hour.
The present invention also provides a kind of preparation method of above-mentioned acetone gas sensor, it is characterized in that, comprising:
The first step: clean alumina ceramic tube, the top layer of described alumina ceramic tube is covered with forked gold electrode, and there is the platinum filament extraction electrode at two ends, dry subsequent use;
Second step: the zinc oxide hollow nanofiber with deionized water furnishing pasty state, is coated with as gas sensitive and is attached on the described alumina ceramic tube of the first step,, process tube core in 500～700 ℃ of sintering;
The 3rd step: heater strip is put into the tube core of the second step gained, according to heater-type device common process weld, encapsulate, electricity is aging, processes the acetone gas sensor.
The present invention utilizes the single shaft method of electrostatic spinning of simple and easy operating to prepare zinc oxide hollow nanometer fibre gas-sensitive material; The gas sensor of this material is highly sensitive to acetone under low working temperature, selectivity good, stability is high, and ethanol, methyl alcohol etc. is not all had obviously response.
Compare with the material of prior art, advantage of the present invention is following:
(1) working temperature reduces; Sensitivity raises: the zinc paste of bibliographical information dumb-bell shape and zinc oxide nano rod reach the sensitivity of the acetone gas of 100ppm when working temperature is 300 ℃ and are respectively 26.1 and 30.4; (referring to document Sens. Actuators B 134,2008,166-170; Sens. Actuators B 143,2009, and 93-98), zinc-oxide film is that about 30 (Vacuum 85,2010, and 101-106), the working temperature of these materials is higher, and energy consumption is bigger to the sensitivity of 100ppm acetone when working temperature is 400 ℃; And the sensitivity to 100ppm acetone under 210-230 ℃ working temperature of the zinc oxide hollow nano-fiber material among the present invention is 67.7.
(2) outstanding to the sensitivity of low concentration acetone gas: the sensitivity to the acetone gas of 1ppm when 300 ℃ of the zinc paste of bibliographical information dumb-bell shape and zinc oxide nano rods is respectively 3.8 and 1.9; (referring to document Sens. Actuators B 134; 2008,166-170; Sens. Actuators B 143,2009, and 93-98), this material acetone to 1ppm under 220 ℃ working temperature has obvious response among the present invention, and sensitivity is 7.1, are higher than document money report.
(3) acetone gas there is good selectivity: bibliographical information CdIn
2O
4Sensitivity to 1000ppm acetone and methyl alcohol is 1.5 near the sensitivity maximum difference, thereby can't carry out selective response.Tested the sensitivity 220 ℃ time of sensitive element that the zinc oxide hollow nano-fiber material makes in the present invention to other gases such as 1-1500ppm acetone, methyl alcohol, ethanol, toluene, carbon monoxide, nitrogen dioxide, ammonia, methane; Wherein, Response to acetone gas is tested atmosphere apparently higher than other; Be other test gas 4-5 doubly, the zinc oxide hollow nanometer fibre gas-sensitive material among this explanation the present invention has good selectivity to acetone.
Description of drawings
Fig. 1 is an acetone gas sensor synoptic diagram.
1 platinum filament extraction electrode, 2 gas sensitives, 3 alumina ceramic tubes, 4 heater strips, 5 gold electrodes.
Fig. 2 is a single shaft electrospinning device work synoptic diagram.
6 high-voltage power supplies, 7 liquid storage pipes, 8 spray silk syringe needles, 9 macromolecules/zinc salt fiber, 10 aluminium foil dash receivers, 11 pumps.
Fig. 3 is a zinc oxide hollow nanofiber XRD figure.
Fig. 4 is a zinc oxide hollow nanofiber field emission scanning electron microscope photo.
Fig. 5 is the sensitivity-working temperature curve of acetone gas sensor.
Fig. 6 is acetone gas sensor response-recovery curve in variable concentrations acetone.
Fig. 7 is an acetone gas sensor selectivity curve.
Fig. 8 is an acetone gas sensor stability curve.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is further specified, but protection scope of the present invention is not limited thereto.
Embodiment 1: acetone gas sensor and preparation method thereof:
A kind of acetone gas sensor adopts the heater-type device architecture, is carrier with the alumina ceramic tube; As shown in Figure 1; Be acetone gas sensor synoptic diagram, the outside surface of alumina ceramic tube 3 is covered with gold electrode 5, and there is platinum filament extraction electrode 1 at two ends; Heater strip 4 is arranged in the alumina ceramic tube 3, gas sensitive 2 is arranged outside the alumina ceramic tube 3.
Described gas sensitive 2 is the zinc oxide hollow nanofiber, and it prepares as follows:
As shown in Figure 2, be single shaft electrospinning device work synoptic diagram, an end of liquid storage pipe 7 connects pump 11; The other end has spray silk syringe needle 8; Spray silk syringe needle 8 is as anode, and aluminium foil dash receiver 10 is as negative electrode, and anode is connected high-voltage power supply 6 with negative electrode; Spray silk syringe needle 8 ejection macromolecule/zinc salt fibers 9, aluminium foil dash receiver 10 receives.Distance between anode and the negative electrode is 20cm.
(1), with the 1g water-soluble high-molecular compound (PVP Mw=1300000) adds the mixed solution 10ml of ethanol and DMF (mass ratio is 1:1), under the room temperature on magnetic stirring apparatus constantly stirring 3-4 hour to solution clarify fully;
(2), the 2g zinc acetate is added the 4ml deionized water for stirring to dissolving, then 4 ml zinc solutions are dropwise added in the settled solution of 10 ml steps (1), make the mixed spinning liquid that evenly promptly forms of solution.
(3), the spinning liquid that step (2) is obtained adds in the liquid storage pipe 7 of above-mentioned single shaft device for spinning; Receive product with aluminium foil as negative electrode, apply 17kV voltage and carry out electrostatic spinning, air themperature 50%; Through after the spinning in 12 hours on minus plate with the composite nano-fiber film of the pbz polymer that obtains; Be placed in the vacuum drying chamber and dried 4 hours down in 90 ℃, 600 ℃ of following sintering were removed macromolecular compound in 3 hours in muffle furnace then, obtained the zinc oxide hollow nanofiber.Fig. 3, Fig. 4 are respectively zinc oxide hollow nanofiber XRD figure and field emission scanning electron microscope photo.
The preparation method of described acetone gas sensor is following:
(1) selecting internal diameter for use is 1.6mm, and external diameter is 2mm, and the alumina ceramic tube that is about 8mm is a carrier, and its top layer is covered with forked gold electrode, and there is the platinum filament extraction electrode at two ends.Clean up with deionized water, dry subsequent use.
(2) take by weighing the zinc oxide hollow nanofiber that about 6mg makes, behind the porphyrize, add small amount of deionized water furnishing pasty state, evenly be coated with and be attached on the above-mentioned alumina ceramic tube.Sensitive layer thickness is in the micron number magnitude.
(3) alumina ceramic tube in (2) is placed sintering 1h in 600 ℃ of muffle furnaces, process tube core.
(4) a nickel chromium triangle heater strip is put into the aforementioned tube in-core; Weld according to heater-type device common process; Platinum filament on electrode lead-in wire and nickel chromium triangle heater strip are welded in respectively on the relevant position of base; At last explosion-proof net is fixed on encapsulated moulding on the base, packaged senser element was carried out electricity aging 240 hours.
The key technical indexes of acetone gas sensor of the present invention is following: sensing range: 1-1500ppm; Working temperature: 210-230 ℃; Detection sensitivity: 7.1-160; Response time :≤17s; Release time :≤15s.
With the performance of the gas-sensitive sensor device of processing with HW-30A type air-sensitive tester test gas-sensitive sensor device, test atmosphere adopts static distribution method to test.Through the adjustment heating power, change working temperature, test the sensitivity to 100ppm acetone under different temperatures of this gas-sensitive sensor device, definition sensitivity be the resistance of gas sensor in normal air with certain density detected gas in the ratio of resistance.As shown in Figure 5, for the sensitivity-working temperature curve of acetone gas sensor, along with the rising of working temperature, the acetone gas sensor also constantly raises to the sensitivity of acetone, reaches maximal value at 220 ℃, and sensitivity subsequently descends.Therefore, this acetone gas sensor is confirmed at 220 ℃ the optimum working temperature scope of acetone.
In 220 ℃ of optimum working temperature scopes, the acetone gas sensor is exposed to its response-recovery characteristic in the acetone test gas of variable concentrations, as shown in Figure 6, the acetone gas sensor is the response-recovery curve in variable concentrations acetone, corresponding acetone concentration 1; 10,20,30,50,70; 100,150, during 200ppm, the sensitivity of this acetone gas sensor is respectively 7.1,19.2; 25.6,32.3,41.3,49.9,67.7; 79.2,87.9, the response time is 11-17s, be 7-15s release time.
Test this acetone gas sensor change of sensitivity situation to testing in the acetone of variable concentrations, ethanol, methyl alcohol, toluene, carbon monoxide, nitrogen dioxide, ammonia, the methane in the time of 220 ℃; As shown in Figure 7; Be acetone gas sensor selectivity curve; As can be seen from the figure far above other test gas (4-5 doubly), have the ability low concentration acetone gas in the environment is carried out selective response by the zinc oxide hollow nanofiber among this explanation the present invention to the sensitivity of acetone for this element.
Test acetone gas sensor in 60 days to 1,10,50,100, the change of sensitivity curve of 200ppm acetone, as shown in Figure 8, be acetone gas sensor stability curve, the sensitivity substantially constant explains that this acetone gas sensor shows good stability.
As stated; Zinc oxide hollow nanometer fibre gas-sensitive material among the present invention can have higher sensitivity to acetone under lower working temperature; Under the situation that other interference gas exist, acetone is carried out selective response, response recovers rapidly and is better stable.Therefore this material is well suited for as acetone air-sensitive material, can be applicable to the acetone in the living environment is monitored.
Claims (10)
1. acetone gas sensor; It is characterized in that; Adopt the zinc oxide hollow nanofiber as gas sensitive; The preparation method of described zinc oxide hollow nanofiber comprises: the spinning solution that will contain zinc salt and high molecular polymer carries out the single shaft electrostatic spinning, oven dry, and the knot that reburns is removed macromolecule wherein.
2. acetone gas sensor as claimed in claim 1; It is characterized in that; The described compound method that contains the spinning solution of zinc salt and high molecular polymer is: with ethanol and N, the dissolving of the mixed solvent of dinethylformamide obtains settled solution, and soluble zinc salt is obtained zinc solution with deionized water dissolving with water-soluble high-molecular compound; The zinc solution of gained is dropwise joined in the above-mentioned settled solution, mix.
3. acetone gas sensor as claimed in claim 2; It is characterized in that; Described water soluble polymer is a polyvinylpyrrolidone, described ethanol and N, ethanol and N in the mixed solvent of dinethylformamide; The mass ratio of dinethylformamide is 1:0.1～10, and the w/v of described water soluble polymer and mixed solvent is 1g:5～10ml.
4. acetone gas sensor as claimed in claim 2 is characterized in that, described soluble zinc salt is a zinc acetate, and the w/v of described soluble zinc salt and deionized water is 1g:1～2.5ml.
5. acetone gas sensor as claimed in claim 2 is characterized in that, the volume ratio of described zinc solution and settled solution is 2:3～10.
6. acetone gas sensor as claimed in claim 1; It is characterized in that; The actual conditions of described single shaft electrostatic spinning is: the spinning solution that will contain zinc salt and high molecular polymer joins in the liquid storage pipe (7) of single shaft electrostatic spinning apparatus, with the spray silk syringe needle (8) of liquid storage pipe (7) as anode, with aluminium foil dash receiver (10) as negative electrode; Distance between anode and the negative electrode is 10～30cm, and the voltage that applies 10～30V carries out the single shaft electrostatic spinning.
7. acetone gas sensor as claimed in claim 6 is characterized in that, the air themperature of described single shaft electrostatic spinning is 45～60%, and the spinning time is 10～14 hours.
8. acetone gas sensor as claimed in claim 1 is characterized in that, the temperature of described oven dry is that 80～100 ℃, time are 3～5 hours.
9. acetone gas sensor as claimed in claim 1 is characterized in that, described sintering temperature is 500～700 ℃, and the time is 1～5 hour.
10. the preparation method of each acetone gas sensor in the claim 1～9 is characterized in that, comprising:
The first step: clean alumina ceramic tube (3), there is platinum filament extraction electrode (1) at the two ends of described alumina ceramic tube, dry subsequent use;
Second step: the zinc oxide hollow nanofiber with deionized water furnishing pasty state, is coated with as gas sensitive (2) and is attached on the described alumina ceramic tube of the first step (3),, process tube core in 500～700 ℃ of sintering;
The 3rd step: heater strip (4) is put into the tube core of the second step gained, according to heater-type device common process weld, encapsulate, electricity is aging, processes the acetone gas sensor.
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| CN103115947A (en) * | 2013-03-05 | 2013-05-22 | 济南大学 | Preparation method and application of carbon-doped mesoporous metal oxide acetone sensor |
| CN103323359A (en) * | 2013-06-09 | 2013-09-25 | 青岛大学 | Method for detecting low-concentration carbon monoxide gas |
| CN103901075A (en) * | 2014-03-13 | 2014-07-02 | 郑州轻工业学院 | Preparation methods for three-dimensional porous ZnO nano sheet ball gas sensitive material and gas sensitive element |
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