CN107884446A - A kind of alcohol gas sensor based on multi-element metal oxide sensitive material - Google Patents
A kind of alcohol gas sensor based on multi-element metal oxide sensitive material Download PDFInfo
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Abstract
The present invention relates to a kind of alcohol gas sensor based on multi-element metal oxide sensitive material, the gas sensor is heater-type structure, including：The alumina ceramic tube, the sensitive material coated in ceramic pipe surface, the nichrome heating coil through earthenware that 2 parallel and discrete annular gold electrodes are come with by outer surface are formed, and two platinum filament pins are connected with each gold electrode；The sensitive material is made up of sensitive material A and sensitive material B mixing, and the sensitive material A is ZnO nano fiber, and the sensitive material B is ternary metal oxide CuZnSnO4Nanorod structure.
Description
Technical field
The present invention relates to alcohol gas sensor technical field, more particularly to one kind to be based on multi-element metal oxide sensitivity material
The alcohol gas sensor of material.
Background technology
Into 21 century, the mankind have stepped into the society of advanced IT application.Sensor technology is as a kind of modernization science and technology
Cutting edge technology, be one of three big pillars of modern information industry.Kind of sensor is various, and sensitive material is sensor production
Core, in recent years, with the continuous development of semi-conducting material, nano material is gradually made the most of the advantage in sensor field.Producing
During the species of the gas used and the gas generated in process of production, quantity also increasing, wherein, many gases are
Inflammable and explosive, or many gases are toxic gases, for the sake of security, just must be to gas in use, transport, storage etc.
Aspect strengthens monitoring, and therefore, in sensor, gas sensor application field is extensive, has a extensive future.
ZnO and SnO2It is the gas sensor sensitive material being developed earliest, its excellent performance, however, single metal
The shortcomings of poor selectivity, operating temperature is high be present in oxide material.Research shows that structure multi-element metal oxide material is to improve
The effective way of sensor gas-sensitive property.
The content of the invention
Based on technical problem set forth above, the present invention is intended to provide a kind of second based on multi-element metal oxide sensitive material
Alcohol gas sensor, to solve problem set forth above.
A kind of alcohol gas sensor based on multi-element metal oxide sensitive material is provided in embodiments of the invention,
The gas sensor is heater-type structure, including：The oxidation of 2 parallel and discrete annular gold electrodes is come with by outer surface
Aluminium earthenware, the sensitive material coated in ceramic pipe surface, the nichrome heating coil through earthenware form, each gold electricity
Two platinum filament pins are connected with extremely；The sensitive material is made up of sensitive material A and sensitive material B mixing, the sensitive material
Material A is ZnO nano fiber, and the sensitive material B is ternary metal oxide CuZnSnO4Nanorod structure.
The technical scheme that embodiments of the invention provide can include the following benefits：
In the alcohol gas sensor of the present invention, by ZnO nano fiber and CuZnSnO4Nanometer rods mixing is used as sensitive material
Material, wherein, the ZnO nano fiber has big specific surface area, and fiber has microcellular structure, using the teaching of the invention it is possible to provide good gas expands
Approach is dissipated, in addition, CuZnSnO4The surface and interface state of material, while each component collaboration hair are added in nanometer rods by doping
The performance for being different from homogenous material is waved, on the basis of each material independence is kept, again with produced by each component synergy
Combination property, substantially increase the performance of sensor.
The additional aspect of the present invention and advantage will be set forth in part in the description, and will partly become from the following description
Obtain substantially, or recognized by the practice of the present invention.It should be appreciated that the general description and following detailed description of the above are only
It is exemplary and explanatory, the present invention can not be limited.
Brief description of the drawings
Using accompanying drawing, the invention will be further described, but the embodiment in accompanying drawing does not form any limit to the present invention
System, for one of ordinary skill in the art, on the premise of not paying creative work, can also be obtained according to the following drawings
Other accompanying drawings.
Fig. 1 is the structural representation of gas sensor described in the embodiment of the present invention.
Embodiment
Here exemplary embodiment will be illustrated in detail, its example is illustrated in the accompanying drawings.Following description is related to
During accompanying drawing, unless otherwise indicated, the same numbers in different accompanying drawings represent same or analogous key element.Following exemplary embodiment
Described in embodiment do not represent and the consistent all embodiments of the present invention.On the contrary, they be only with it is such as appended
The example of the consistent apparatus and method of some aspects being described in detail in claims, of the invention.
Embodiments of the invention are related to a kind of alcohol gas sensor based on multi-element metal oxide sensitive material, such as scheme
Shown in 1, the gas sensor is heater-type structure, including：2 parallel and discrete annular gold electrodes are come with by outer surface
11 alumina ceramic tube 12, the sensitive material 13 coated in the surface of earthenware 12, the nichrome through earthenware 12 heat
Coil 14 is formed, and two platinum filament pins are connected with each gold electrode 11.
Wherein, the sensitive material 13 is made up of sensitive material A and sensitive material B mixing, and the sensitive material A is ZnO
Nanofiber, the sensitive material B are ternary metal oxide CuZnSnO4Nanorod structure；
Specifically, the ZnO nano fiber is to be prepared by polyvinyl alcohol and zinc nitrate using method of electrostatic spinning；It is described
CuZnSnO4Nanometer rods are to pass through SnCl4·5H2O、Zn(NO3)2·6H2O、Cu(NO3)2·3H2Prepared by O hydro-thermal methods.
In above-mentioned sensitive material, sensitive material A is ZnO nano fiber, and sensitive material B is CuZnSnO4Nanometer rods, this hair
Bright technical scheme is by ZnO nano fiber and CuZnSnO4Nanometer rods mixing is used as sensitive material, wherein, ZnO nano fiber tool
There is big specific surface area, and fiber has microcellular structure, using the teaching of the invention it is possible to provide good gas dispensing path, in addition, CuZnSnO4Receive
The surface and interface state of material is added in rice rod by doping, while each component collaboration plays the property for being different from homogenous material
Can, on the basis of each material independence is kept, again with combination property caused by each component synergy, substantially increase
The performance of sensor.
Preferably, in sensitive material, the mass ratio of the sensitive material A and sensitive material B are 5:1.
By the way that in above-mentioned sensitive material, sensitive material A, B mass ratio control are 5:1 so that the alcohol gas sense
Device greatly improves to the detection sensitivity of ethanol, serves unexpected technique effect.
In above-mentioned sensitive material, sensitive material A is ZnO nano fiber, and the ZnO nano fiber is electrostatic spinning legal system
Standby, its average diameter is 230nm.
ZnO is the n-type semiconductor material with wide forbidden band for having wurtzite structure, and it is in optics, electricity, catalysis etc. performance
Uniqueness, practical application is suffered from fields such as sensor, solar cell, lithium battery, catalysis.Particularly in gas sensor side
Face.At present, the research to zno-based gas sensor mainly takes the mode such as nanostructured control, doping, compound raising property
Energy；Meanwhile electrostatic spinning is a kind of short-cut method for preparing nano material, and the technology on zinc oxide gas sensor at present
In scheme, it is few as the technical scheme of sensitive material that zinc oxide nano fiber is prepared using method of electrostatic spinning；The technology of the present invention
In scheme, ZnO nano fiber and CuZnSnO prepared by method of electrostatic spinning4Nanometer rods mix the sensitive material as sensor,
Because the ZnO nano fiber has big specific surface area, and fiber has microcellular structure, can ensure CuZnSnO4Nanometer rods are filled
Divide and be integrated into ZnO nano fiber, thus obtained sensor has the advantages of sensitivity is high, response is rapid.
When the ZnO nano average fibre diameter is 230nm so that detection spirit of the alcohol gas sensor to ethanol
Sensitivity greatly improves, and serves unexpected technique effect.
In above-mentioned sensitive material, sensitive material B is CuZnSnO4Nanometer rods, the nanorod diameter are 40nm, length
For 120nm.
As described above, ZnO is one of metal oxide gas sensitive developed earliest, but in practical application, the material is deposited
Poor selectivity, operating temperature is high the problems such as.And be to improve the main method of the material-sensitive performance by doping, in the present invention
CuZnSnO4Nanometer rods, Zn, Sn, Cu element are combined, construct ternary metal oxide composite, composite tool
There are good physics and chemical stability, Zn, Sn, Cu element are combined, and good selectivity can be showed gas.
Above-mentioned sensitive material A preparation process is：
Step 1, first, it is respectively 4.6g, 50g to take the quality of polyvinyl alcohol and distilled water, mixing, obtains mixed solution,
It is stirred vigorously at 80 DEG C, is mixed uniformly, zinc nitrate is then added into mixed solution, is continued to stir 4h, obtain mixed solution
A；
Step 2, above-mentioned mixed solution A is fitted into spinneret pipe, using copper wire as positive pole, aluminium foil is as the negative of receiver board
Pole, the voltage applied during electrostatic spinning is 16kV, and the distance between spinning head and receiver board are 19.5cm, carries out electrostatic
Spinning, composite fibre is obtained, gained composite fibre fiber is put into vacuum drying chamber and is dried for standby；
Step 3, the composite fibre of above-mentioned drying is put into high temperature resistance furnace and sintered in air atmosphere, at 800 DEG C
5h is calcined, to remove high-molecular polyivnyl alcohol, ZnO nano fiber is obtained after natural cooling.
Above-mentioned sensitive material B preparation process is：
Step 1, Cu (NO are taken3)2·3H2O、Zn(NO3)2·6H2O、SnCl4·5H2O is 10mmol, is mixed and is dissolved in
In deionized water, mixed solution, magnetic agitation 2h are formed；
Step 2,0.2M NaOH solution is added into above-mentioned mixed solution, regulation pH value is 12, obtains mixed solution B, so
After transfer them in autoclave, react 14h at 200 DEG C；
Step 3, after reaction terminates, mixed solution B is taken out into reactor, at room temperature natural cooling；Then by reaction product
Centrifugation, washing, dry 20h, finally by dried powder in O at 80 DEG C2The 2h that annealed under atmosphere, under the conditions of 516 DEG C is obtained
Final product, as CuZnSnO4Nanometer rods.
And then by ZnO nano fiber obtained above, CuZnSnO4Nanometer rods are 5 according to mass ratio:1 ratio mixing
Uniformly, ethanol is then added, is modulated into pasty slurry, by it coated on earthenware, is dried after slurry solidification at 96 DEG C
5h, sensitive material 13 is obtained, and then obtain the gas sensor.
Reference examples 1
A kind of alcohol gas sensor based on multi-element metal oxide sensitive material, the gas sensor are heater-type
Structure, including：The alumina ceramic tube 12 of 2 parallel and discrete annular gold electrodes 11 is come with, coated in pottery by outer surface
The sensitive material 13 on the surface of porcelain tube 12, the nichrome heating coil 14 through earthenware 12 form, and connect on each gold electrode 11
It is connected to two platinum filament pins.
Wherein, the sensitive material 13 is made up of sensitive material A and sensitive material B mixing, and the sensitive material A is ZnO
Nanofiber, the sensitive material B are ternary metal oxide CuZnSnO4Nanorod structure；In sensitive material, the sensitivity
Materials A and sensitive material B mass ratio are 5:1.
Specifically, the ZnO nano fiber is to be prepared by polyvinyl alcohol and zinc nitrate using method of electrostatic spinning, it is flat
A diameter of 230nm.
Above-mentioned sensitive material A preparation process is：
Step 1, first, it is respectively 4.6g, 50g to take the quality of polyvinyl alcohol and distilled water, mixing, obtains mixed solution,
It is stirred vigorously at 80 DEG C, is mixed uniformly, zinc nitrate is then added into mixed solution, is continued to stir 4h, obtain mixed solution
A；
Step 2, above-mentioned mixed solution A is fitted into spinneret pipe, using copper wire as positive pole, aluminium foil is as the negative of receiver board
Pole, the voltage applied during electrostatic spinning is 16kV, and the distance between spinning head and receiver board are 19.5cm, carries out electrostatic
Spinning, composite fibre is obtained, gained composite fibre fiber is put into vacuum drying chamber and is dried for standby；
Step 3, the composite fibre of above-mentioned drying is put into high temperature resistance furnace and sintered in air atmosphere, at 800 DEG C
5h is calcined, to remove high-molecular polyivnyl alcohol, ZnO nano fiber is obtained after natural cooling.
The CuZnSnO4Nanometer rods are to pass through SnCl4·5H2O、Zn(NO3)2·6H2O、Cu(NO3)2·3H2O hydro-thermal methods
Prepare, the nanorod diameter is 40nm, length 120nm.
Above-mentioned sensitive material B preparation process is：
Step 1, Cu (NO are taken3)2·3H2O、Zn(NO3)2·6H2O、SnCl4·5H2O is 10mmol, is mixed and is dissolved in
In deionized water, mixed solution, magnetic agitation 2h are formed；
Step 2,0.2M NaOH solution is added into above-mentioned mixed solution, regulation pH value is 12, obtains mixed solution B, so
After transfer them in autoclave, react 14h at 200 DEG C；
Step 3, after reaction terminates, mixed solution B is taken out into reactor, at room temperature natural cooling；Then by reaction product
Centrifugation, washing, dry 20h, finally by dried powder in O at 80 DEG C2The 2h that annealed under atmosphere, under the conditions of 516 DEG C is obtained
Final product, as CuZnSnO4Nanometer rods.
And then by ZnO nano fiber obtained above, CuZnSnO4Nanometer rods are 5 according to mass ratio:1 ratio mixing
Uniformly, ethanol is then added, is modulated into pasty slurry, by it coated on earthenware, is dried after slurry solidification at 96 DEG C
5h, sensitive material 13 is obtained, and then obtain the gas sensor.
The operating temperature of metal-oxide semiconductor (MOS) sensitive material is to weigh an important parameter of sensor performance, air-sensitive
Test temperature is defined as optimum working temperature when element reaches highest to the responsiveness for testing gas.
Surveyed therefore, sensor obtained above is respectively placed under the conditions of 200 DEG C, 230 DEG C, 260 DEG C, 290 DEG C, 320 DEG C
The sensitivity to 100ppm ethanol is tried, as a result such as following table：
| Operating temperature | 200℃ | 230℃ | 260℃ | 290℃ | 320℃ |
| Sensitivity | 6 | 17 | 31 | 43 | 19 |
Understanding, sensor of the present invention raises with the rise sensitivity of temperature, reaches highest in 290 DEG C of sensitivity, with
Begun to decline afterwards with the further rise of temperature, sensitivity.
In order to test selectivity of the sensor of the present invention to alcohol gas, in the case where temperature is 290 DEG C, put respectively
In 100ppm ethanol, methanol, acetone, toluene, its sensitivity is tested, as a result such as following table：
| Gas type | Ethanol | Methanol | Acetone | Toluene |
| Sensitivity | 42 | 35 | 16 | 19 |
It can be seen that at identical temperature, in above-mentioned ethanol, methanol, acetone, toluene, spirit of the sensor to ethanol
Sensitivity highest, it has good selectivity to ethanol.
Reference examples 2
A kind of alcohol gas sensor based on multi-element metal oxide sensitive material, the gas sensor are heater-type
Structure, including：The alumina ceramic tube 12 of 2 parallel and discrete annular gold electrodes 11 is come with, coated in pottery by outer surface
The sensitive material 13 on the surface of porcelain tube 12, the nichrome heating coil 14 through earthenware 12 form, and connect on each gold electrode 11
It is connected to two platinum filament pins.
Wherein, the sensitive material 13 is made up of sensitive material A and sensitive material B mixing, and the sensitive material A is ZnO
Nanofiber, the sensitive material B are ternary metal oxide CuZnSnO4Nanorod structure；In sensitive material, the sensitivity
Materials A and sensitive material B mass ratio are 3:1.
Specifically, the ZnO nano fiber is to be prepared by polyvinyl alcohol and zinc nitrate using method of electrostatic spinning, it is flat
A diameter of 130nm.
Above-mentioned sensitive material A preparation process is：
Step 1, first, it is respectively 4.6g, 50g to take the quality of polyvinyl alcohol and distilled water, mixing, obtains mixed solution,
It is stirred vigorously at 80 DEG C, is mixed uniformly, zinc nitrate is then added into mixed solution, is continued to stir 4h, obtain mixed solution
A；
Step 2, above-mentioned mixed solution A is fitted into spinneret pipe, using copper wire as positive pole, aluminium foil is as the negative of receiver board
Pole, the voltage applied during electrostatic spinning is 14kV, and the distance between spinning head and receiver board are 18.4cm, carries out electrostatic
Spinning, composite fibre is obtained, gained composite fibre fiber is put into vacuum drying chamber and is dried for standby；
Step 3, the composite fibre of above-mentioned drying is put into high temperature resistance furnace and sintered in air atmosphere, at 800 DEG C
5h is calcined, to remove high-molecular polyivnyl alcohol, ZnO nano fiber is obtained after natural cooling.
The CuZnSnO4Nanometer rods are to pass through SnCl4·5H2O、Zn(NO3)2·6H2O、Cu(NO3)2·3H2O hydro-thermal methods
Prepare, the nanorod diameter is 40nm, length 120nm.
Above-mentioned sensitive material B preparation process is：
Step 1, Cu (NO are taken3)2·3H2O、Zn(NO3)2·6H2O、SnCl4·5H2O is 10mmol, is mixed and is dissolved in
In deionized water, mixed solution, magnetic agitation 2h are formed；
Step 2,0.2M NaOH solution is added into above-mentioned mixed solution, regulation pH value is 12, obtains mixed solution B, so
After transfer them in autoclave, react 14h at 200 DEG C；
Step 3, after reaction terminates, mixed solution B is taken out into reactor, at room temperature natural cooling；Then by reaction product
Centrifugation, washing, dry 20h, finally by dried powder in O at 80 DEG C2The 2h that annealed under atmosphere, under the conditions of 516 DEG C is obtained
Final product, as CuZnSnO4Nanometer rods.
And then by ZnO nano fiber obtained above, CuZnSnO4Nanometer rods are 3 according to mass ratio:1 ratio mixing
Uniformly, ethanol is then added, is modulated into pasty slurry, by it coated on earthenware, is dried after slurry solidification at 96 DEG C
5h, sensitive material 13 is obtained, and then obtain the gas sensor.
The operating temperature of metal-oxide semiconductor (MOS) sensitive material is to weigh an important parameter of sensor performance, air-sensitive
Test temperature is defined as optimum working temperature when element reaches highest to the responsiveness for testing gas.
Surveyed therefore, sensor obtained above is respectively placed under the conditions of 200 DEG C, 230 DEG C, 260 DEG C, 290 DEG C, 320 DEG C
The sensitivity to 100ppm ethanol is tried, as a result such as following table：
| Operating temperature | 200℃ | 230℃ | 260℃ | 290℃ | 320℃ |
| Sensitivity | 4 | 14 | 27 | 39 | 15 |
Understanding, sensor of the present invention raises with the rise sensitivity of temperature, reaches highest in 290 DEG C of sensitivity, with
Begun to decline afterwards with the further rise of temperature, sensitivity.
In order to test selectivity of the sensor of the present invention to alcohol gas, in the case where temperature is 290 DEG C, put respectively
In 100ppm ethanol, methanol, acetone, toluene, its sensitivity is tested, as a result such as following table：
| Gas type | Ethanol | Methanol | Acetone | Toluene |
| Sensitivity | 27 | 21 | 13 | 12 |
It can be seen that at identical temperature, in above-mentioned ethanol, methanol, acetone, toluene, spirit of the sensor to ethanol
Sensitivity highest, but the selectivity to ethanol is not fine.
Pass through the contrast of reference examples 1 and reference examples 2, it can be seen that in the sensitive material of the sensor, sensitive material A,
B mass ratio, ZnO nano average fibre diameter has a great influence to the sensor relative to the sensitivity of alcohol gas；When
Sensitive material A, B mass ratio control are 5:1, and, when the ZnO nano average fibre diameter is 230nm, it has to ethanol
There are good sensitivity and selectivity.
The preferred mode of the present invention is the foregoing is only, is not intended to limit the invention, it is all in the spiritual and former of the present invention
Within then, any modification, equivalent substitution and improvements made etc., it should be included in the scope of the protection.
Claims (8)
1. a kind of alcohol gas sensor based on multi-element metal oxide sensitive material, the gas sensor is heater-type knot
Structure, including：The alumina ceramic tube of 2 parallel and discrete annular gold electrodes is come with, coated in earthenware table by outer surface
The sensitive material in face, the nichrome heating coil through earthenware are formed, and two platinum filament pins are connected with each gold electrode；
Characterized in that, the sensitive material is made up of sensitive material A and sensitive material B mixing, the sensitive material A is ZnO nano
Fiber, the sensitive material B are ternary metal oxide CuZnSnO4Nanorod structure.
2. alcohol gas sensor according to claim 1, it is characterised in that in sensitive material, the sensitive material A and
Sensitive material B mass ratio is 5:1.
3. alcohol gas sensor according to claim 1, it is characterised in that the ZnO nano fiber is by poly- second
What enol and zinc nitrate were prepared using method of electrostatic spinning.
4. alcohol gas sensor according to claim 3, it is characterised in that the ZnO nano average fibre diameter is
230nm。
5. alcohol gas sensor according to claim 4, it is characterised in that the preparation process of the sensitive material A is：
Step 1, first, it is respectively 4.6g, 50g to take the quality of polyvinyl alcohol and distilled water, mixing, mixed solution is obtained, at 80 DEG C
Under be stirred vigorously, be mixed uniformly, zinc nitrate is then added into mixed solution, continue stir 4h, obtain mixed solution A；
Step 2, above-mentioned mixed solution A is fitted into spinneret pipe, using copper wire as positive pole, negative pole of the aluminium foil as receiver board,
The voltage applied during electrostatic spinning is 16kV, and the distance between spinning head and receiver board are 19.5cm, carries out Static Spinning
Silk, obtains composite fibre, gained composite fibre fiber is put into vacuum drying chamber and is dried for standby；
Step 3, the composite fibre of above-mentioned drying is put into high temperature resistance furnace and sintered in air atmosphere, calcined at 800 DEG C
5h, to remove high-molecular polyivnyl alcohol, ZnO nano fiber is obtained after natural cooling.
6. alcohol gas sensor according to claim 1, it is characterised in that the CuZnSnO4Nanometer rods are to pass through
SnCl4·5H2O、Zn(NO3)2·6H2O、Cu(NO3)2·3H2Prepared by O hydro-thermal methods.
7. alcohol gas sensor according to claim 6, it is characterised in that the CuZnSnO4Nanorod diameter be 40~
60nm, length 120nm.
8. alcohol gas sensor according to claim 7, it is characterised in that the preparation process of the sensitive material B is：
Step 1, Cu (NO are taken3)2·3H2O、Zn(NO3)2·6H2O、SnCl4·5H2O is 10mmol, be mixed be dissolved in from
In sub- water, mixed solution, magnetic agitation 2h are formed；
Step 2,0.2M NaOH solution is added into above-mentioned mixed solution, regulation pH value is 12, obtains mixed solution B, then will
It is transferred in autoclave, reacts 14h at 200 DEG C；
Step 3, after reaction terminates, mixed solution B is taken out into reactor, at room temperature natural cooling；Then reaction product is centrifuged,
Washing, 20h is dried at 80 DEG C, finally by dried powder in O2The 2h that annealed under atmosphere, under the conditions of 516 DEG C is finally produced
Thing, as CuZnSnO4Nanometer rods.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112964754A (en) * | 2021-02-09 | 2021-06-15 | 上海应用技术大学 | Synthetic method of flexible ethanol sensor |
| CN113189152A (en) * | 2021-04-30 | 2021-07-30 | 重庆文理学院 | Sensing equipment capable of detecting ethanol in high-temperature environment and processing method |
| CN114354724A (en) * | 2022-01-11 | 2022-04-15 | 山西大学 | Metal oxide semiconductor gas sensor and preparation method and application thereof |
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