CN104931540A - Gas sensor array and preparation method thereof - Google Patents
Gas sensor array and preparation method thereof Download PDFInfo
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- CN104931540A CN104931540A CN201410105900.2A CN201410105900A CN104931540A CN 104931540 A CN104931540 A CN 104931540A CN 201410105900 A CN201410105900 A CN 201410105900A CN 104931540 A CN104931540 A CN 104931540A
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- metal oxide
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Abstract
The invention discloses a gas sensor array and a preparation method thereof. The gas sensor array is prepared from a single-type semiconductor metal oxide nano material. In the preparation method, a semiconductor metal oxide gas-sensitive material is taken as the raw material, a layer-layer assembly mode is adopted, and multiple gas sensors containing gas sensitive membranes with different thicknesses are produced so as to form a sensor array. The responding to gas of each gas sensor is different, and thus the gas selectivity of the gas sensor array is greatly improved. The prepared sensor array can recognize and differentiate a plurality of organic volatile gases with a poisonous concentration.
Description
Technical field
The present invention relates to a kind of gas sensor array, build the method for gas sensor array specifically with single metal oxide semiconductor nano material.
Background technology
Gas sensor based on metal oxide semiconductor, due to advantages such as its volume is little, energy consumption is low, good stabilities, has been widely used in the multiple fields such as industry, environmental monitoring, food inspection.But this gas sensor almost has response to multiple gases, when detecting mixed gas or having interference gas existence etc., be difficult to effectively identify target components.
Different gas sensors is formed an array, utilize it to the intersection information of gas with various response, improve the selectivity of sensor, be considered to a kind of well means.The simplest method is with SnO by different
2based on commercialization gas sensor composition sensor array, but this sensor array is to the recognition capability of gas, is still limited to limited commercialization gas sensor.Some noble metals although adulterate in gas sensitive, as Ag, Pd, Pt, Au etc., can improve sensor to a certain extent to the response of gas and selectivity.But limited metal oxide semiconductor gas sensitive, and single doping way, do not make the selective problems of sensor fundamentally well be promoted.
Summary of the invention
Based on above problem, the object of the present invention is to provide a kind of array gas sensor and preparation method thereof, using single metal oxide semiconductor as gas sensitive, prepare the air-sensitive film of different-thickness, build different gas sensors, and form array.
For achieving the above object, the technical solution used in the present invention is:
Form array by N number of gas sensor, N be greater than 1 positive integer; Each sensor all adopts metal oxide semiconductor nano material of the same race to be sensing membrane, and in each sensor, the thickness of sensing membrane is different, and then different to gas with various response, detects with the differentiation realizing gas.
Described metal oxide semiconductor of the same race is SnO
2, ZnO, In
2o
3, CuO, CdO, Fe
2o
3, TiO
2, WO
3or the one in NiO metal oxide.
Described nano material is nano particle, nano wire, nanobelt, nanotube, nano-pore micron film, nano-pore micron tube, nano-pore micro wire wherein one or more.
Single-sensor adopts layer-layer construction from part preparation, and concrete steps are as follows:
1) the metal oxide semiconductor nano material of getting certain mass evenly spreads in organic solvent;
2) the scattered metal oxide semiconductor nano material described in certain volume step 1) is got, drop in N number of ceramic pipe on the surface, ceramic pipe with certain rotating speed around axial rotation, metal oxide semiconductor nano material homogeneous dispersion is made to be spin-coated on its surface, until organic solvent volatilizees completely, form layer of semiconductor metal oxide film; Different ceramic pipe drips the metal oxide semiconductor nano material of different number of times, obtain multiple metal oxide semiconductor film with the different number of plies;
3) in step 2) described in each ceramic pipe surface tumble in two wires, wire contacts with metal oxide semiconductor film; A heater strip is placed in ceramic pipe; Two wires are connected with metering circuit respectively, and heater strip is connected with heater circuit, form N number of sensor; Sensor works at 350 DEG C, and resistance is at 0.05 ~ 5000K Ω;
4) by N number of sensor arrangement composition metal oxide semiconductor gas sensor array.
The quality of described metal oxide semiconductor nano material is 5 ~ 200mg, and ultrasonic disperse forms suspension in the organic solvent of 1 ~ 100mL.
Described organic solvent is one or more in ethanol, ethylene glycol, acetone, toluene, chloroform, normal hexane, acetonitrile, butanone.
Described rotating speed is 2-100rpm.
Tool of the present invention has the following advantages:
1. the present invention only adopts a kind of Metal oxide semiconductor gas-sensitiveness material to build sensor array, no longer can be limited to the commercialization semiconductor gas sensor of limited kinds on market;
2. because the response of metal oxide semiconductor gas sensor affects by many factors, as the electronic conduction situation difference between Metal oxide semiconductor gas-sensitiveness material layer, gas spreads the decline of rate of diffusion and the concentration caused between the different layers, metal oxide semiconductor material pore size, metal oxide semiconductor contact resistance etc.Therefore, along with the increase of the number of plies, the response of metal oxide semiconductor gas sensor to gas is not linear increasing, thus result in the difference that every sensor responds gas;
3., because every gas sensor is all different to the response of VOCs gas, the selectivity of sensor array to gas is improved greatly;
4. this sensor and preparation method thereof is simple and reliable, has good practicality.
Accompanying drawing explanation
Fig. 1 (a) is In
2o
3nano-pore micron tube sensor array measures the fingerprint base of the multiple volatile organic compounds of intoxicating concentration;
Fig. 1 (b) is the classification of unknown sample in fingerprint base.
Fig. 2 (a) is SnO
2the fingerprint base of the multiple volatile organic compounds of nanowire sensor array measurement intoxicating concentration;
Fig. 2 (b) is the classification of unknown sample in fingerprint base.
Embodiment
Form array by N number of gas sensor, N be greater than 1 positive integer; Each sensor all adopts metal oxide semiconductor (SnO of the same race
2, ZnO, In
2o
3, CuO, CdO, Fe
2o
3, TiO
2, WO
3or the one in NiO metal oxide) nano material (nano particle, nano wire, nanobelt, nanotube, nano-pore micron film, nano-pore micron tube, nano-pore micro wire wherein one or more) is sensing membrane, in each sensor, the thickness of sensing membrane is different, different to gas with various response, and then the differentiation realizing gas detects.
Single-sensor adopts layer-layer construction from part to prepare gas sensor, and concrete steps are as follows:
1) a kind of metal oxide semiconductor nano material being got 5 ~ 200mg evenly spreads in the organic solvent (in ethanol, ethylene glycol, acetone, toluene, chloroform, normal hexane, acetonitrile, butanone one or more) of 1 ~ 100mL;
2) the scattered metal oxide semiconductor nano material described in certain volume step 1) is got, drop in N number of ceramic pipe on the surface, ceramic pipe with 2-100rpm rotating speed around axial rotation, metal oxide semiconductor nano material homogeneous dispersion is made to be spin-coated on its surface, until organic solvent volatilizees completely, form layer of semiconductor metal oxide film; Different ceramic pipe drips the metal oxide semiconductor nano material of different number of times, obtain multiple metal oxide semiconductor film with the different number of plies;
3) in step 2) described in each ceramic pipe surface tumble in two wires, wire contacts with metal oxide semiconductor film; A heater strip is placed in ceramic pipe; Two wires are connected with metering circuit respectively, and heater strip is connected with heater circuit, form N number of sensor; Sensor works at 350 DEG C, and resistance is at 0.05 ~ 5000K Ω;
4) by N number of sensor arrangement composition metal oxide semiconductor gas sensor array.
Embodiment 1:
1) by In
2o
3metal oxide evenly spreads in the ethanol of 20mL containing the nano-pore micron tube 10mg of nano-pore;
2) In that 5 μ L are scattered is got
2o
3metal oxide nano hole micron tube material, drop in 1 ceramic pipe on the surface, ceramic pipe around axial rotation, makes In with 20rpm rotating speed
2o
3metal oxide nano-material homogeneous dispersion is spin-coated on its surface, until organic solvent volatilizees completely, forms layer of semiconductor In
2o
3metal oxide film; Different ceramic pipe drips 5 μ L semiconductor In of different number of times
2o
3metal oxide nano-material, obtains the semiconductor In that 16 have the different number of plies
2o
3metal oxide film;
3) two wires are tumbled on each ceramic pipe surface, wire and semiconductor In
2o
3metal oxide film contacts; A heater strip is placed in ceramic pipe; Two wires are connected with metering circuit respectively, and heater strip is connected with heater circuit, form 16 sensors; Sensor is under 350 DEG C of heating conditions, and resistance is at 0.05 ~ 5000K Ω; By 16 sensor arrangement composition conductor oxidate gas sensor arrays.
The response of definition sensor is S=R
a/ R
g, wherein R
afor the aerial resistance of sensor, R
gfor the resistance of sensor in gas to be measured.
The gas sensor of 16 above-mentioned preparations is built sensor array, for the multiple concentration known (dangerous concentrations of US Occupational Safety health research defined, be divided into IDLH(excessive risk) and PEL(low-risk) two kinds of concentration) sensing of various criterion volatile organic compounds, often kind of gas does five parallel experiments, " fingerprint base " is built, as shown in Fig. 1 (a) with the response gathered.Determine methyl alcohol (6000ppm, IDLH concentration altogether, 200ppm, PEL concentration), ethanol (3300ppm, IDLH concentration, 1000ppm, PEL concentration), isopropyl alcohol (2000ppm, IDLH concentration, 400ppm, PEL concentration), acetone (2500ppm, IDLH concentration, 1000ppm, PEL concentration), ethyl acetate (2000ppm, IDLH concentration, 400ppm, PEL concentration), normal butyl alcohol (1400ppm, IDLH concentration, 100ppm, PEL concentration), acetic acid (50ppm, IDLH concentration, 10ppm, PEL concentration), formaldehyde (20ppm, IDLH concentration), o-xylene (900ppm, IDLH concentration), 1, 2, 4-trimethylbenzene (135ppm, IDLH concentration) 17 kinds of concentration of ten kinds of gases, construct " fingerprint base ", adopting SPSS(StatisticalPackage for the Social Sciences) mathematical statistics method analysis show that in " fingerprint base ", each concentration all can be separated with other gas zone, and self five Duplicate Samples can overlap (not marking in figure) completely, the reappearance that sensor has had and excellent separating capacity are absolutely proved.Simultaneously, the fingerprint that unknown gas gathers is compared with this " fingerprint base ", as shown in Fig. 1 (b), same employing SPSS mathematical statistics method carries out classification analysis, from classification analysis, unknown gas and ethyl acetate rely on recently, and show that unknown gas is ethyl acetate, and its concentration close to or exceed the 400ppm value of regulation.
Embodiment 2:
1) by SnO
2metal oxide nano-wire 10mg evenly spreads in the acetone of 20mL;
2) SnO that 5 μ L are scattered is got
2metal oxide nano-wire material, drops in 1 ceramic pipe on the surface, and ceramic pipe around axial rotation with 20rpm rotating speed, makes homogeneous dispersion be spin-coated on its surface, until organic solvent volatilizees completely, forms layer of semiconductor metal oxide film; Different ceramic pipe drips 5 μ L metal oxide semiconductor nano materials of different number of times, obtain the metal oxide semiconductor film that 16 have the different number of plies;
3) tumble in two wires on each ceramic pipe surface, wire contacts with metal oxide semiconductor film; A heater strip is placed in ceramic pipe; Two wires are connected with metering circuit respectively, and heater strip is connected with heater circuit, form 16 sensors; Sensor is under 350 DEG C of heating conditions, and resistance is at 0.05 ~ 5000K Ω; By 16 sensor arrangement composition conductor oxidate gas sensor arrays.
The response of definition sensor is S=R
a/ R
g, wherein R
afor the aerial resistance of sensor, R
gfor the resistance of sensor in gas to be measured.
The gas sensor of 16 above-mentioned preparations is built sensor array, for the multiple concentration known (dangerous concentrations of US Occupational Safety health research defined, be divided into IDLH(excessive risk) and PEL(low-risk) two kinds of concentration) sensing of various criterion volatile organic compounds, often kind of gas does five parallel experiments, " fingerprint base " is built, as shown in Figure 2 (a) shows with the response gathered.Determine formaldehyde (0.75ppm, PEL concentration) altogether, o-xylene (100ppm, PEL concentration), 1,2,4-trimethylbenzene (27ppm, PEL concentration), toluene (500ppm, IDLH concentration; 200ppm, PEL concentration), ethylbenzene (800ppm, IDLH concentration; 100ppm, PEL concentration), acetonitrile (500ppm, IDLH concentration; 40ppm, PEL concentration), chloroform (500ppm, IDLH concentration; 50ppm, PEL concentration) 11 kinds of concentration of seven kinds of gases and blank, construct " fingerprint base ", adopting SPSS(StatisticalPackage for the Social Sciences) mathematical statistics method analysis show that in " fingerprint base ", each concentration all can be separated with other gas zone, and self five Duplicate Samples can overlap (not marking in figure) completely, has absolutely proved the reappearance that sensor has had and excellent separating capacity.Simultaneously, the fingerprint that unknown gas gathers and " fingerprint base " are compared, as shown in Fig. 2 (b), same employing SPSS mathematical statistics method carries out classification analysis, from classification analysis, unknown gas and formaldehyde rely on recently, and show that unknown gas is formaldehyde, its concentration close to or exceed the 0.75ppm value of regulation.
Claims (7)
1. a gas sensor array, is characterized in that:
Form array by N number of gas sensor, N be greater than 1 positive integer; Each sensor all adopts metal oxide semiconductor nano material of the same race to be sensing membrane, and in each sensor, the thickness of sensing membrane is different, and then different to gas with various response, detects with the differentiation realizing gas.
2. according to sensor array according to claim 1, it is characterized in that: described metal oxide semiconductor is SnO
2, ZnO, In
2o
3, CuO, CdO, Fe
2o
3, TiO
2, WO
3or the one in NiO metal oxide.
3. according to sensor array according to claim 1, it is characterized in that: described nano material is nano particle, nano wire, nanobelt, nanotube, nano-pore micron film, nano-pore micron tube, nano-pore micro wire wherein one or more.
4. a preparation method for gas sensor array as claimed in claim 1, is characterized in that: single-sensor adopts layer-layer construction from part preparation, and concrete steps are as follows:
1) the metal oxide semiconductor nano material of getting certain mass evenly spreads in organic solvent;
2) the scattered metal oxide semiconductor nano material described in certain volume step 1) is got, drop in N number of ceramic pipe on the surface, ceramic pipe with certain rotating speed around axial rotation, metal oxide semiconductor nano material homogeneous dispersion is made to be spin-coated on its surface, until organic solvent volatilizees completely, form layer of semiconductor metal oxide film; Different ceramic pipe drips the metal oxide semiconductor nano material dispersion liquid of different number of times, obtain multiple metal oxide semiconductor film with the different number of plies;
3) in step 2) described in each ceramic pipe surface tumble in two wires, wire contacts with metal oxide semiconductor film; A heater strip is placed in ceramic pipe; Two wires are connected with metering circuit respectively, and heater strip is connected with heater circuit, form N number of sensor; Sensor works at 350 DEG C, and resistance is at 0.05 ~ 5000K Ω;
4) by N number of sensor arrangement composition metal oxide semiconductor gas sensor array.
5. according to preparation method according to claim 4, it is characterized in that: the quality of described metal oxide semiconductor nano material is 5 ~ 200mg, and ultrasonic disperse forms suspension in the organic solvent of 1 ~ 100mL.
6. according to preparation method according to claim 4, it is characterized in that: described organic solvent is one or more in ethanol, ethylene glycol, acetone, toluene, chloroform, normal hexane, acetonitrile, butanone.
7. according to preparation method according to claim 4, it is characterized in that: described rotating speed is 2-100rpm.
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| CN106158743A (en) * | 2016-05-20 | 2016-11-23 | 上海申矽凌微电子科技有限公司 | Utilize the manufacture method of the sensor of many inducing pixels detection multiple gases |
| CN106546637A (en) * | 2016-11-08 | 2017-03-29 | 吉林大学 | A kind of ethyl acetate gas sensor and preparation method thereof |
| CN107037177A (en) * | 2016-02-03 | 2017-08-11 | 中国科学院大连化学物理研究所 | Plus alkali improves Colorimetric gas sensor to Cl2The method of detection sensitivity |
| CN108051422A (en) * | 2017-11-21 | 2018-05-18 | 复旦大学 | A kind of trace explosive and drug detector and its application method |
| CN108088955A (en) * | 2017-11-30 | 2018-05-29 | 苏州慧闻纳米科技有限公司 | A kind of anti-interference gas sensor |
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| CN106128004A (en) * | 2016-07-19 | 2016-11-16 | 中国民航大学 | Fire detector based on array gas sensor |
| CN106546637B (en) * | 2016-11-08 | 2018-12-21 | 吉林大学 | A kind of ethyl acetate gas sensor and preparation method thereof |
| CN106546637A (en) * | 2016-11-08 | 2017-03-29 | 吉林大学 | A kind of ethyl acetate gas sensor and preparation method thereof |
| CN108051422B (en) * | 2017-11-21 | 2020-09-29 | 复旦大学 | Trace explosive and drug detector and using method thereof |
| CN108051422A (en) * | 2017-11-21 | 2018-05-18 | 复旦大学 | A kind of trace explosive and drug detector and its application method |
| CN109839408A (en) * | 2017-11-24 | 2019-06-04 | 中国科学院大连化学物理研究所 | It is a kind of using nanocomposite as the ammonia gas sensor of sensing membrane |
| CN108088955A (en) * | 2017-11-30 | 2018-05-29 | 苏州慧闻纳米科技有限公司 | A kind of anti-interference gas sensor |
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Application publication date: 20150923 |