CN102661977A - Sensitive material for benzene vapor detecting sensor and preparation method of gas sensor - Google Patents
Sensitive material for benzene vapor detecting sensor and preparation method of gas sensor Download PDFInfo
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- CN102661977A CN102661977A CN2012101670410A CN201210167041A CN102661977A CN 102661977 A CN102661977 A CN 102661977A CN 2012101670410 A CN2012101670410 A CN 2012101670410A CN 201210167041 A CN201210167041 A CN 201210167041A CN 102661977 A CN102661977 A CN 102661977A
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Abstract
The invention relates to a sensitive material for a benzene vapor detecting sensor and a preparation method of a gas sensor and belongs to the technical field of function materials, sensing technology and environmental monitoring technology. The preparation method includes: using SnO2 prepared by a sol-gel method and commercial V2O5 to prepare a composite material by means of solid-phase reaction, and using the composite material as the sensitive material to detect benzene vapor; subjecting the gas sensor coated with the SnO2/V2O5 nano-composite material to calcination at 500 DEG C, and welding the gas sensor according to a thick-film semiconductor gas sensor manufacture process, namely, welding a quadrangular electrode lead platinum filament; and ageing and packaging after drying so that the gas sensor for detecting benzene vapor is prepared. The prepared gas sensor for detecting the benzene vapor has the advantages of high sensitivity, high selectivity, low power consumption and the like, and can be used for detecting benzene vapor and methylbenzene vapor in the atmosphere or indoor environment.
Description
Technical field
The present invention relates to the preparation method of a kind of benzene vapor detecting sensor sensitive material and gas sensor, function of dominant material, sensing technology and environmental monitoring technology field.
Background technology
Benzene is a kind of colourless, pleasantly sweet transparency liquid at normal temperatures, and has strong aromatic odor, and boiling point is 80.1 ℃.It is insoluble in water, is soluble in organic solvent, and itself also is widely used in aspects such as the glue that uses in various building materialss and the interior decoration, coating, leather and fur products as organic solvent.As everyone knows, benzene is very large to the harm of human body, is just confirmed as strong carcinogen by the World Health Organization (WHO) many years ago, so the concentration of benzene vapor is not only necessaryly in the monitoring of environmental, also is necessary.Many countries with the detection of benzene vapor as an important indicator in the Indoor Environment Detection.The benzene vapor detecting sensor of having reported has quartzy crystallite balance detection method, photoelectric sensor, electrochemical sensor, LB film sensors, gas chromatography sensor, infrared detector and carbon nano tube sensor etc.; But all exist some inevitable shortcomings; Huge like equipment, inconvenience is carried; Complex equipments, maintenance cost is high; Organic sensitive material is synthetic complicated, and productive rate is not high; Detect lower limit and do not reach the Indoor Environment Detection standard; Made of carbon nanotubes is complicated, and is noble metal decorated, causes material cost more high.
Summary of the invention
To the defective that prior art exists, the purpose of this invention is to provide the preparation method of a kind of benzene vapor detecting sensor sensitive material and gas sensor.Semiconductor gas sensor is because advantages such as cost is low, easy to carry, low in energy consumption, sensitivity height all are people's research focuses all the time.Develop outstanding benzene vapor detecting sensor and will make important contribution, to ensureing that human health also has significant meaning for environmental monitoring, scientific-technical progress and academic research.
For achieving the above object, the present invention adopts following technical scheme:
The preparation method of a kind of benzene vapor detecting sensor sensitive material and gas sensor has following preparation process and step:
A. SnO
2The preparation of nano material: with SnCl
45H
2O is a raw material, is dissolved in the solution of processing 0.05-0.2 mol/L in the deionized water, 40 ℃ of water bath with thermostatic control magnetic agitation 30-50 minute, and it is 2-5 that dropping ammonia is adjusted to pH; Obtain white gelatinous precipitate after the centrifuging, then with deionized water and absolute ethyl alcohol centrifuge washing repeatedly, obtain gel particle after the drying,, use the agate mortar porphyrize, promptly get SnO 500 ℃ of annealing in process 2 hours
2Nano material;
B. SnO
2/ V
2O
5The preparation of nano composite material: with SnO
2: V
2O
5By mass ratio was that 99:1-4:1 grinds two kinds of nano materials evenly after mixing, and obtained SnO at 600 ℃ of following solid phase reaction 2-3 hours
2/ V
2O
5Nano composite material, i.e. benzene vapor detecting sensor sensitive material;
C. the preparation of benzene vapor detecting sensor gas sensor: earlier benzene vapor detecting sensor sensitive material is placed mortar, behind the adding small amount of deionized water furnishing pasty state, be evenly coated on the four angle plane substrates, after 500 ℃ of cured 2-3 hours; By thick film semiconducting gas sensor manufacture craft gas sensor is welded, i.e. the welding of four electrical leads platinum filaments; After the infrared lamp drying, on agingtable, wear out, encapsulate, promptly make benzene vapor detecting sensor gas sensor.
Compared with prior art, the advantage of the benzene vapor detecting sensor sensitive material of the present invention's preparation and gas sensor is following:
1, preparation technology is simple, environmental friendliness, and organic solvent-free, cost is low, is easy to realize mass production.
2, the sensor gas sensor adopts a certain amount of V
2O
5With SnO
2The nano material composite methods improves sensitivity and the selectivity of gas sensitive to benzene vapor.
3, adopt thick-film type gas sensor element preparation technology, effectively reduce the working temperature and the power consumption of element, and effectively reduced the volume of element, realized portability and low-power consumption.
Description of drawings
Fig. 1 is the SnO of the inventive method preparation
2The x-ray diffraction pattern of nano material.
Fig. 2 is the SnO of the inventive method preparation
2The transmission electron microscope photo of nano material.
Fig. 3 is the SnO of the inventive method preparation
2/ V
2O
5The x-ray diffraction pattern of nano composite material.
Fig. 4 is the SnO of the inventive method preparation
2/ V
2O
5The transmission electron microscope photo of nano composite material.
Fig. 5 is the gas sensor that the makes response recovery curve figure to 50 ppm ethanol, methyl alcohol, acetone, formaldehyde, benzene and toluene.
Fig. 6 is the gas sensor that the makes response recovery curve figure to benzene vapor in 0.5 ppm to the 200 ppm scope.
Embodiment
Below in conjunction with accompanying drawing as follows to specific embodiment narration of the present invention:
Embodiment one
The preparation method of benzene vapor detecting sensor sensitive material and gas sensor may further comprise the steps in this example:
A. SnO
2The preparation of nano material: with SnCl
45H
2O is a raw material, is dissolved in the solution of processing 0.05mol/L in the deionized water, 40 ℃ of water bath with thermostatic control magnetic agitation 30 minutes, and it is 2-5 that dropping ammonia is adjusted to pH; Obtain white gelatinous precipitate after the centrifuging, then with deionized water and absolute ethyl alcohol centrifuge washing repeatedly, obtain gel particle after the drying,, use the agate mortar porphyrize, promptly get SnO 500 ℃ of annealing in process 2 hours
2Nano material;
B. SnO
2/ V
2O
5The preparation of nano composite material: with SnO
2: V
2O
5By mass ratio is that 99:1 grinds two kinds of nano materials evenly after mixing, and obtains SnO in 2 hours 600 ℃ of following solid phase reactions
2/ V
2O
5Nano composite material, i.e. benzene vapor sensor sensing material;
C. the preparation of benzene vapor detecting sensor gas sensor: earlier benzene vapor sensor sensing material is placed mortar, add small amount of deionized water furnishing pasty state after, be evenly coated in four angle plane substrates, through 500 ℃ of cured after 2 hours; By thick film semiconducting gas sensor manufacture craft gas sensor is welded (i.e. the welding of four electrical leads platinum filaments); After the infrared lamp drying, on agingtable, wear out, encapsulation promptly makes benzene vapor and detects the detecting sensor gas sensor.
Embodiment two
The preparation method of benzene vapor detecting sensor sensitive material and gas sensor may further comprise the steps in this example:
A. SnO
2The preparation of nano material: with SnCl
45H
2O is a raw material, is dissolved in the solution of processing 0.1 mol/L in the deionized water, 40 ℃ of water bath with thermostatic control magnetic agitation 40 minutes, and it is 2-5 that dropping ammonia is adjusted to pH; Obtain white gelatinous precipitate after the centrifuging, then with deionized water and absolute ethyl alcohol centrifuge washing repeatedly, obtain gel particle after the drying,, use the agate mortar porphyrize, promptly get SnO 500 ℃ of annealing in process 2 hours
2Nano material;
B. SnO
2/ V
2O
5The preparation of nano composite material: with SnO
2: V
2O
5By mass ratio is that 9:1 grinds two kinds of nano materials evenly after mixing, and obtains SnO in 3 hours 600 ℃ of following solid phase reactions
2/ V
2O
5Nano composite material, i.e. benzene vapor sensor sensing material;
C. the preparation of benzene vapor detecting sensor gas sensor: earlier benzene vapor sensor sensing material is placed mortar, add small amount of deionized water furnishing pasty state after, be evenly coated in four angle plane substrates, through 500 ℃ of cured after 2 hours; By thick film semiconducting gas sensor manufacture craft gas sensor is welded (i.e. the welding of four electrical leads platinum filaments); After the infrared lamp drying, on agingtable, wear out, encapsulation promptly makes benzene vapor and detects the detecting sensor gas sensor.
Embodiment three
The preparation method of benzene vapor detecting sensor sensitive material and gas sensor may further comprise the steps in this example:
A. SnO
2The preparation of nano material: with SnCl
45H
2O is a raw material, is dissolved in the solution of processing 0.2 mol/L in the deionized water, 40 ℃ of water bath with thermostatic control magnetic agitation 50 minutes, and it is 2-5 that dropping ammonia is adjusted to pH; Obtain white gelatinous precipitate after the centrifuging, then with deionized water and absolute ethyl alcohol centrifuge washing repeatedly, obtain gel particle after the drying,, use the agate mortar porphyrize, promptly get SnO 500 ℃ of annealing in process 2 hours
2Nano material;
B. SnO
2/ V
2O
5The preparation of nano composite material: with SnO
2: V
2O
5By mass ratio is that 4:1 grinds two kinds of nano materials evenly after mixing, and obtains SnO in 3 hours 600 ℃ of following solid phase reactions
2/ V
2O
5Nano composite material, i.e. benzene vapor sensor sensing material;
C. the preparation of benzene vapor detecting sensor gas sensor: earlier benzene vapor sensor sensing material is placed mortar, add small amount of deionized water furnishing pasty state after, be evenly coated in four angle plane substrates, through 500 ℃ of cured after 2 hours; By thick film semiconducting gas sensor manufacture craft gas sensor is welded (i.e. the welding of four electrical leads platinum filaments); After the infrared lamp drying, on agingtable, wear out, encapsulation promptly makes benzene vapor and detects the detecting sensor gas sensor.
The material list air-sensitive test result of seeking peace
To the air-sensitive test that prepared material among the embodiment two carries out each item sign and gas sensor is carried out, the result is following:
The thing of gained monomer material and compound substance characterizes through X-ray diffraction and transmission electron microscope: the diffraction peak of X-ray diffraction is mainly tetragonal crystal system SnO among Fig. 1
2(JCPDS 41-1445); Can find out prepared SnO on Fig. 2 transmission electron microscope photo
2Be nano material, particle diameter is tens nanometers; X-ray diffraction pattern among Fig. 3 is found out the SnO that has tetragonal crystal system in the compound substance
2(JCPDS 41-1445) and rhombic V
2O
5(JCPDS 41-1426) two phases explain that the two is a compound substance, and can SnO on the transmission electron microscope photo among Fig. 4
2/ V
2O
5Nano composite material is comparatively uniform nano particle.
The test of the air-sensitive of gas sensor is carried out on the WS-30A test macro: can find out in the multiple gases response recovery curve of gas sensor that embodiment obtains referring to Fig. 5 50 ppm, and the highest to the response of benzene vapor, and also corresponding release time is all very short.Done special test to the variable concentrations benzene vapor among Fig. 6, detected lower limit at 0.5-1ppm, responsiveness is along with the increase of benzene vapor concentration progressively increases, and corresponding release time is all in 10 seconds.
Claims (1)
1. the preparation method of benzene vapor detecting sensor sensitive material and gas sensor is characterized in that having following preparation process and step:
A. SnO
2The preparation of nano material: with SnCl
45H
2O is a raw material, is dissolved in the solution of processing 0.05-0.2 mol/L in the deionized water, 40 ℃ of water bath with thermostatic control magnetic agitation 30-50 minute, and it is 2-5 that dropping ammonia is adjusted to pH; Obtain white gelatinous precipitate after the centrifuging, then with deionized water and absolute ethyl alcohol centrifuge washing repeatedly, obtain gel particle after the drying,, use the agate mortar porphyrize, promptly get SnO 500 ℃ of annealing in process 2 hours
2Nano material;
B. SnO
2/ V
2O
5The preparation of nano composite material: with SnO
2: V
2O
5By mass ratio was that 99:1-4:1 grinds two kinds of nano materials evenly after mixing, and obtained SnO at 600 ℃ of following solid phase reaction 2-3 hours
2/ V
2O
5Nano composite material, i.e. benzene vapor detecting sensor sensitive material;
C. the preparation of benzene vapor detecting sensor gas sensor: earlier benzene vapor detecting sensor sensitive material is placed mortar, behind the adding small amount of deionized water furnishing pasty state, be evenly coated on the four angle plane substrates, after 500 ℃ of cured 2-3 hours; By thick film semiconducting gas sensor manufacture craft gas sensor is welded, i.e. the welding of four electrical leads platinum filaments; After the infrared lamp drying, on agingtable, wear out, encapsulate, promptly make benzene vapor detecting sensor gas sensor.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103207220A (en) * | 2013-03-08 | 2013-07-17 | 武汉工程大学 | Benzene gas sensitive material and preparation method thereof as well as manufacturing method of benzene gas sensitive device |
| CN104132987A (en) * | 2014-05-30 | 2014-11-05 | 中国石油化工股份有限公司 | Preparation method for gas-sensitive element for hydrocarbon gas detection |
| CN104267022A (en) * | 2014-09-04 | 2015-01-07 | 北京联合大学 | Cross sensitive material of ammonia and benzene in air and preparation method of cross sensitive material |
| KR101813226B1 (en) | 2016-11-21 | 2018-01-02 | 고려대학교 산학협력단 | Benzene gas sensors using catalytic overlayer structured oxide semiconductors and fabrication method thereof |
Citations (2)
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|---|---|---|---|---|
| CN1041453A (en) * | 1989-07-29 | 1990-04-18 | 吉林大学 | Ethanol, nitrogen dioxide double sensitive film air sensor for both gases |
| US20100043529A1 (en) * | 2008-08-20 | 2010-02-25 | Ce Wang | Nanofibers and methods of making same and using same in humidity sensors |
-
2012
- 2012-05-28 CN CN201210167041.0A patent/CN102661977B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1041453A (en) * | 1989-07-29 | 1990-04-18 | 吉林大学 | Ethanol, nitrogen dioxide double sensitive film air sensor for both gases |
| US20100043529A1 (en) * | 2008-08-20 | 2010-02-25 | Ce Wang | Nanofibers and methods of making same and using same in humidity sensors |
Non-Patent Citations (2)
| Title |
|---|
| 《功能材料与器材学报》 20110430 李建昌等 "金属氧化物半导体薄膜气敏机理研究进展" 第205-217页 1 第17卷, 第2期 * |
| 李建昌等: ""金属氧化物半导体薄膜气敏机理研究进展"", 《功能材料与器材学报》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103207220A (en) * | 2013-03-08 | 2013-07-17 | 武汉工程大学 | Benzene gas sensitive material and preparation method thereof as well as manufacturing method of benzene gas sensitive device |
| CN103207220B (en) * | 2013-03-08 | 2015-05-20 | 武汉工程大学 | Benzene gas sensitive material and preparation method thereof as well as manufacturing method of benzene gas sensitive device |
| CN104132987A (en) * | 2014-05-30 | 2014-11-05 | 中国石油化工股份有限公司 | Preparation method for gas-sensitive element for hydrocarbon gas detection |
| CN104267022A (en) * | 2014-09-04 | 2015-01-07 | 北京联合大学 | Cross sensitive material of ammonia and benzene in air and preparation method of cross sensitive material |
| KR101813226B1 (en) | 2016-11-21 | 2018-01-02 | 고려대학교 산학협력단 | Benzene gas sensors using catalytic overlayer structured oxide semiconductors and fabrication method thereof |
| WO2018093235A1 (en) * | 2016-11-21 | 2018-05-24 | 고려대학교 산학협력단 | Benzene gas sensor using multilayered sensitive film structure and method for manufacturing same |
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