CN102331443B - Acetone gas sensor and manufacturing method thereof - Google Patents
Acetone gas sensor and manufacturing method thereof Download PDFInfo
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- CN102331443B CN102331443B CN 201110195804 CN201110195804A CN102331443B CN 102331443 B CN102331443 B CN 102331443B CN 201110195804 CN201110195804 CN 201110195804 CN 201110195804 A CN201110195804 A CN 201110195804A CN 102331443 B CN102331443 B CN 102331443B
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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-shaped semiconductor material, has been used as at present a kind of high-performance gas sensitive and has been widely used in NO
2, H
2S, NH
3High-sensitivity detection etc. various toxic and harmfuls.Since S.Iijima found carbon nano-tube 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, nanobelt), 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 the existing tension force in surface and viscoelasticity power under high-voltage electric field, carries out the stretch bending campaign and obtains nanometer to the technology of Sub-micro Fibers.This technology has that equipment is simple, and production cost is low, uses material extensively to reach the advantages such as specific surface area is large.At present, have the report that utilizes the coaxial electrostatic spinning equipment to prepare the hollow metal oxide both at home and abroad, but the coaxial electrostatic spinning equipment is comparatively complicated, all there are difficulty in the selection of solvent and the setting of spinning parameter.The single shaft Static Spinning has then overcome above deficiency.
At present mainly concentrate on ZnO, SnO with oxide as the sensitive material research of acetone steam
2, CeO
2, the 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 larger; 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 lowest detectable limit 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 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, with the aluminium foil dash receiver 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.
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 for subsequent use;
Second step: the zinc oxide hollow nanofiber with deionized water furnishing pasty state, is coated on the described alumina ceramic tube of the first step as gas sensitive, in 500～700 ℃ of sintering, makes tube core;
The 3rd step: heater strip is put into the tube core of second step gained, according to heater-type device common process weld, encapsulate, electricity is aging, makes 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 that this material is made is highly sensitive to acetone under low working temperature, selectivity good, stability is high, and ethanol, methyl alcohol etc. are all responded without obvious.
Compare with the material of prior art, advantage of the present invention is as follows:
(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 larger 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 in the present invention the sensitivity to other gases such as 1-1500ppm acetone, methyl alcohol, ethanol, toluene, carbon monoxide, nitrogen dioxide, ammonia, methane 220 ℃ time of sensitive element that the zinc oxide hollow nano-fiber material makes, wherein, response to acetone gas is tested atmosphere apparently higher than other, be the 4-5 of other test gas 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 the 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 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 zinc oxide hollow nanofiber XRD figure.
Fig. 4 is 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 the acetone gas sensor selectivity curve.
Fig. 8 is the acetone gas sensor stability curve.
Embodiment
The present invention will be further described below in conjunction with drawings and Examples, but protection scope of the present invention is not limited to this.
Embodiment 1: acetone gas sensor and preparation method thereof:
A kind of acetone gas sensor, adopt the heater-type device architecture, take alumina ceramic tube as carrier, as shown in Figure 1, be the 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 is prepared as follows:
As shown in Figure 2, be single shaft electrospinning device work synoptic diagram, one 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), 1g water-soluble high-molecular compound (PVP, Mw=1300000) is added ethanol and the DMF(mass ratio is 1:1) mixed solution 10ml, on magnetic stirring apparatus, constantly stir under the room temperature and clarified fully to solution in 3-4 hour;
(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 namely 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 under 90 ℃, then 600 ℃ of lower sintering were removed macromolecular compound in 3 hours in muffle furnace, 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 as follows:
(1) selecting internal diameter is 1.6mm, and external diameter is 2mm, and the alumina ceramic tube that is about 8mm is 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 for subsequent use.
(2) take by weighing the zinc oxide hollow nanofiber that about 6mg makes, behind the porphyrize, add a small amount of deionized water furnishing pasty state, evenly be coated 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, make 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 as follows: sensing range: 1-1500ppm; Working temperature: 210-230 ℃; Detection sensitivity: 7.1-160; Response time :≤17s; Release time :≤15s.
With the performance that the gas-sensitive sensor device of making is tested gas-sensitive sensor device with HW-30A type air-sensitive tester, test atmosphere adopts static distribution method to test.By adjusting 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 detection gas in the ratio of resistance.As shown in Figure 5, for the sensitivity of acetone gas sensor-working temperature curve, along with the rising of working temperature, acetone gas sensor also constantly raises to the sensitivity of acetone, reaches maximal value at 220 ℃, and subsequently sensitivity descends.Therefore, this acetone gas sensor is determined at 220 ℃ the optimum working temperature scope of acetone.
In 220 ℃ of optimum working temperature scopes, acetone gas sensor is exposed to its response-recovery characteristic in the acetone test gas of variable concentrations, as shown in Figure 6, 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, and 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 the 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.
The test acetone gas sensor to the change of sensitivity curve of 1,10,50,100,200ppm acetone, as shown in Figure 8, was the acetone gas sensor stability curve in 60 days, the sensitivity substantially constant illustrates that this acetone gas sensor shows good stability.
As mentioned above, zinc oxide hollow nanometer fibre gas-sensitive material among the present invention can have higher sensitivity to acetone under lower working temperature, in 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 (3)
1. the preparation method of an acetone gas sensor comprises:
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 for subsequent use;
Second step: the zinc oxide hollow nanofiber with deionized water furnishing pasty state, is coated on the described alumina ceramic tube of the first step (3) as gas sensitive (2), in 500～700 ℃ of sintering, makes tube core;
The 3rd step: heater strip (4) is put into the tube core of second step gained, according to heater-type device common process weld, encapsulate, electricity is aging, makes acetone gas sensor;
It is characterized in that 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; The described compound method that contains the spinning solution of zinc salt and high molecular polymer is: with water-soluble high-molecular compound ethanol and N, the mixed solvent dissolving of dinethylformamide 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 polyvinylpyrrolidone, described ethanol and N, the mass ratio of ethanol and DMF is 1:0.1～10 in the mixed solvent of dinethylformamide, and the w/v of described water soluble polymer and mixed solvent is 1g:5～10ml; Described soluble zinc salt is zinc acetate, and the w/v of described soluble zinc salt and deionized water is 1g:1～2.5ml; The volume ratio of described zinc solution and settled solution is 2:3～10; 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; The temperature of described oven dry is that 80～100 ℃, time are 3～5 hours; Described sintering temperature is 500～700 ℃, and the time is 1～5 hour.
2. the preparation method of acetone gas sensor as claimed in claim 1 is characterized in that, the air humidity of described single shaft electrostatic spinning is 45～60%, and the spinning time is 10～14 hours.
3. the acetone gas sensor of preparation method's preparation of adopting claim 1-2.
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| CN103115947B (en) * | 2013-03-05 | 2014-04-23 | 济南大学 | Preparation method and application of carbon-doped mesoporous metal oxide acetone sensor |
| CN103323359B (en) * | 2013-06-09 | 2015-11-04 | 青岛大学 | A kind of detection method of Low Level Carbon Monoxide gas |
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| CN104458815A (en) * | 2014-12-11 | 2015-03-25 | 郑州大学 | High-molecular gas sensitive material as well as preparation method and application thereof |
| CN104502417A (en) * | 2015-01-10 | 2015-04-08 | 吉林大学 | La2O3-WO3 oxide semiconductor acetone gas sensor and preparation method thereof |
| CN104819999B (en) * | 2015-05-05 | 2017-10-24 | 太原理工大学 | The preparation method of alcohol gas sensor element with super fast response recovery characteristics |
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| CN107884447A (en) * | 2017-11-07 | 2018-04-06 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of perovskite acetone sensing material and products thereof and application |
| CN109781797A (en) * | 2019-03-13 | 2019-05-21 | 珠海格力电器股份有限公司 | TVOC gas sensing devices, air processor |
| CN112391698B (en) * | 2019-08-19 | 2022-10-11 | Tcl科技集团股份有限公司 | Nano material and preparation method thereof and quantum dot light-emitting diode |
| CN113406155B (en) * | 2021-06-23 | 2022-08-05 | 长春理工大学 | Tin oxide/polyacid/tungsten oxide three-layer coaxial nanofiber gas sensing material and preparation method thereof |
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