CN106053549B - It is a kind of for detecting the gas sensitive of low concentration acetone - Google Patents
It is a kind of for detecting the gas sensitive of low concentration acetone Download PDFInfo
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- CN106053549B CN106053549B CN201610384382.1A CN201610384382A CN106053549B CN 106053549 B CN106053549 B CN 106053549B CN 201610384382 A CN201610384382 A CN 201610384382A CN 106053549 B CN106053549 B CN 106053549B
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- acetone
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
Abstract
The invention discloses a kind of for detecting the gas sensitive of low concentration acetone, belongs to gas sensitive technical field.Gas sensitive composition is graphene quantum dot-SnO2, in which: the quality of graphene quantum dot accounts for the 5-15% of gas sensitive gross mass.Using the material as heater-type gas sensor made of sensitive material, under 270 DEG C of operating temperatures, to the sensitivity of 0.1ppm acetone (component resistance ratio in component resistance and tested gas in air) between 1.2-1.5, to the sensitivity of 1000ppm acetone between 100-140.Response recovery time is respectively less than 50s, which is below 4.1 to the sensitivity of the formaldehyde of 1000ppm, ethyl alcohol, toluene, benzene, front three amine gas under identical operating temperature, therefore the quick detection to low concentration acetone in air may be implemented.
Description
Technical field
The invention belongs to gas sensitive technical fields, and in particular in a kind of pair of air low concentration acetone have it is highly sensitive and
The preferably gas sensitive of selectivity.
Technical background
Acetone is a kind of colourless transparent liquid, there is special acrid odors.Industrially mainly as solvent for explosive,
In the industries such as plastics, rubber, fiber, process hides, grease, spray painting, synthesis ketenes, aceticanhydride, iodoform, polyisoprene rubber also can be used as
The important source material of the substances such as glue, methyl methacrylate, chloroform, epoxy resin.Acetone Central nervous system has inhibition, anesthesia
Effect, high concentration contact the damage that one or two people are likely to occur with liver, kidney and pancreas.China provides working place and residential area
The limit value of acetone in air is 400mg/m respectively3(about 168ppm) and 0.8mg/m3(about 0.34ppm).At present third in measurement air
The method of ketone concentration mainly uses gas chromatography, and this method needs instrument and equipment costly, sampling analysis need to expend compared with
For a long time.
Summary of the invention
In order to overcome the deficiencies of the prior art, the technical problem to be solved in the present invention is to provide a kind of gas sensitive, the materials
Can be used for making the gas sensor of gas sensor, manufactured gas sensor to low concentration acetone in air have it is highly sensitive and
Preferably selectivity.
In order to solve the above technical problems, the present invention is achieved by the following technical programs.
The present invention provides a kind of for detecting the gas sensitive of low concentration acetone, and the gas sensitive is by SnO2And graphene
Quantum dot composition, in which: the quality of graphene quantum dot accounts for the 5-15% of gas sensitive gross mass.
The preparation method and process of the graphene quantum dot are: firstly, 1.0800g graphite oxide is scattered in 80mL diformazan
Ultrasound 30min in base formamide (DMF).Then, mixture is transferred to 200 DEG C of reactions in polytetrafluoroethylene (PTFE) stainless steel cauldron
8h.It is cooled to room temperature, is filtered with 0.22 μm of the filter membrane in aperture, filtered brown filtrate is the graphene amount that contains after reacting
The solution of son point, it is stand-by to collect brown filtrate.
Graphene quantum dot-the SnO2Composite material preparation process is: the graphene quantum dot solution of different volumes point
Dissipate formation 40mL solution, ultrasonic 30min in DMF.0.7012g is analyzed into pure SnCl simultaneously4·5H2O and 0.2402g urea adds
Enter into above-mentioned solution ultrasound 30min.This solution is finally transferred in 50mL polytetrafluoroethylene (PTFE) stainless steel autoclave 160 DEG C,
10h.Reaction is completed to be cooled to room temperature, and product deionized water and dehydrated alcohol filtration washing five times obtain after 80 DEG C of dry 12h
Graphene quantum dot-SnO2Nanocomposite.
Material of the invention can be used as the sensitive material of acetone gas sensing element, make heater-type gas using the material
The method of quick element is: slurry is made in 0.1 gram of material and 0.5 gram of terpinol mixed grinding, slurry is coated onto oxygen with small brushes
Change the surface of aluminium ceramic tube；The size of alumina ceramic tube is: it is 6 millimeters long, 1.6 millimeters of internal diameter, and 2 millimeters of outer diameter, in aluminium oxide
Pipe both ends gold medal makees electrode, spun gold is welded on electrode as lead, distance is 1 millimeter between electrode；It is put in alumina tube
Nichrome wire is set as heater strip, can control aluminium oxide by controlling the electric current for flowing through heater strip and heater strip both end voltage
The temperature of pipe surface sensitive material；The alumina tube for being coated with sensitive material slurry is placed under infrared lamp and is dried to get indirect heat is arrived
Formula gas sensor.Element is that at the working temperature, resistance and element are being tested element in air to the sensitivity of certain gas
The ratio of resistance in gas.
Compared with prior art, the present invention has following technical effect that
1, the present invention is by hydro-thermal reaction method in SnO2In graphene-doped quantum dot composite material is made, with the material work
For heater-type gas sensor made of sensitive material, the quick detection of low concentration acetone in air may be implemented.
2, the gas sensitive has highly sensitive and preferable selectivity to low concentration acetone in air.Using the material as sensitivity
Heater-type gas sensor made of material, when operating temperature is 270 DEG C, element reaches 1000ppm acetone up to sensitivity
100-140 reaches 1.2-1.5 to the sensitivity of 0.1ppm acetone gas, and to the response of 0.1-1000ppm acetone gas and
Recovery time is no more than 25s and 50s respectively.The element under identical operating temperature to the formaldehyde of 1000ppm, ethyl alcohol, toluene,
The sensitivity of benzene, front three amine gas is below 4.1.
Specific embodiment
The present invention is described in detail below in conjunction with specific embodiment, but the present invention is not limited to following embodiments.
Embodiment 1
Formation 40mL solution, ultrasonic 30min in 35mL DMF are dispersed by 5mL graphene quantum dot solution.By 0.7012g
Analyze pure SnCl4·5H2O and 0.2402g urea is added to ultrasound 30min in above-mentioned solution.This solution is finally transferred to 50mL
160 DEG C in polytetrafluoroethylene (PTFE) stainless steel autoclave, 10h.Reaction is completed to be cooled to room temperature, by product deionized water and dehydrated alcohol
Filtration washing five times, graphene quantum dot-SnO is obtained after 80 DEG C of dry 12h2Nanocomposite.Through thermogravimetric analysis composite wood
Graphene quantum dot content is 5%wt in material.
Heater-type element is made in material, measures element under 270 DEG C of operating temperatures to 0.1,1,10,100,1000ppm
The maximum sensitivity of acetone gas is respectively 1.2,5.4,29,78,100.To the acetone response time of 0.1-1000pp and recovery
Time is no more than 20 seconds and 45 seconds.The element is under identical operating temperature to the formaldehyde of 1000ppm, ethyl alcohol, toluene, benzene, front three
The sensitivity of amine gas is below 3.5.
Embodiment 2
Formation 40mL solution, ultrasonic 30min in 30mL DMF are dispersed by 10mL graphene quantum dot solution.It will
0.7012g analyzes pure SnCl4·5H2O and 0.2402g urea is added to ultrasound 30min in above-mentioned solution.Finally this solution is turned
160 DEG C are moved in 50mL polytetrafluoroethylene (PTFE) stainless steel autoclave, 10h.Reaction is completed to be cooled to room temperature, by product deionized water and
Dehydrated alcohol filtration washing five times, graphene quantum dot-SnO is obtained after 80 DEG C of dry 12h2Nanocomposite.Through thermogravimetric point
Analysing graphene quantum dot content in composite material is 9%wt.
Heater-type element is made in material, measures element under 270 DEG C of operating temperatures to 0.1,1,10,100,1000ppm
The maximum sensitivity of acetone gas is respectively 1.5,7.4,33,91,140.To the acetone response time of 0.1-1000pp and recovery
Time is no more than 25 seconds and 50 seconds.The element is under identical operating temperature to the formaldehyde of 1000ppm, ethyl alcohol, toluene, benzene, front three
The sensitivity of amine gas is below 4.1.
Embodiment 3
Formation 40mL solution, ultrasonic 30min in 28mL DMF are dispersed by 12mL graphene quantum dot solution.It will
0.7012g analyzes pure SnCl4·5H2O and 0.2402g urea is added to ultrasound 30min in above-mentioned solution.Finally this solution is turned
160 DEG C are moved in 50mL polytetrafluoroethylene (PTFE) stainless steel autoclave, 10h.Reaction is completed to be cooled to room temperature, by product deionized water and
Dehydrated alcohol filtration washing five times, graphene quantum dot-SnO is obtained after 80 DEG C of dry 12h2Nanocomposite.Through thermogravimetric point
Analysing graphene quantum dot content in composite material is 11%wt.
Heater-type element is made in material, measures element under 270 DEG C of operating temperatures to 0.1,1,10,100,1000ppm
The maximum sensitivity of acetone gas is respectively 1.4,7.0,30,86,123.To the acetone response time of 0.1-1000pp and recovery
Time is no more than 23 seconds and 48 seconds.The element is under identical operating temperature to the formaldehyde of 1000ppm, ethyl alcohol, toluene, benzene, front three
The sensitivity of amine gas is below 3.8.
Embodiment 4
Formation 40mL solution, ultrasonic 30min in 24mL DMF are dispersed by 16mL graphene quantum dot solution.It will
0.7012g analyzes pure SnCl4·5H2O and 0.2402g urea is added to ultrasound 30min in above-mentioned solution.Finally this solution is turned
160 DEG C are moved in 50mL polytetrafluoroethylene (PTFE) stainless steel autoclave, 10h.Reaction is completed to be cooled to room temperature, by product deionized water and
Dehydrated alcohol filtration washing five times, graphene quantum dot-SnO is obtained after 80 DEG C of dry 12h2Nanocomposite.Through thermogravimetric point
Analysing graphene quantum dot content in composite material is 15%wt.
Heater-type element is made in material, measures element under 270 DEG C of operating temperatures to 0.1,1,10,100,1000ppm
The maximum sensitivity of acetone gas is respectively 1.3,6.7,28,80,112.To the acetone response time of 0.1-1000pp and recovery
Time is no more than 23 seconds and 50 seconds.The element is under identical operating temperature to the formaldehyde of 1000ppm, ethyl alcohol, toluene, benzene, front three
The sensitivity of amine gas is below 3.7.
Claims (1)
1. a kind of for detecting the gas sensitive of low concentration acetone, which is characterized in that the gas sensitive is by SnO2And graphene quantum
Point composition, in which: the quality of graphene quantum dot accounts for the 5-15% of gas sensitive gross mass；
The preparation method of the gas sensitive is: dispersing formation 40mL solution in DMF, ultrasound for graphene quantum dot solution
30min；0.7012g is analyzed into pure SnCl simultaneously4·5H2O and 0.2402g urea is added to ultrasound 30min in above-mentioned solution；Most
This solution is transferred to 160 DEG C of reaction 10h in 50mL polytetrafluoroethylene (PTFE) stainless steel autoclave afterwards；Reaction is completed to be cooled to room temperature, will
Product washs, after 80 DEG C of dry 12h to obtain the final product.
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| CN106053549B true CN106053549B (en) | 2019-02-19 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106770466A (en) * | 2016-11-30 | 2017-05-31 | 庞倩桃 | Enhanced gas sensor of a kind of iron oxide quantum dot and preparation method thereof |
| CN106770498B (en) * | 2017-01-12 | 2019-03-05 | 吉林大学 | Acetone sensor, the preparation method and application of rhodium doped stannic oxide nanometer fiber sensitive material based on electrostatic spinning technique preparation |
| CN107121454B (en) * | 2017-04-17 | 2019-08-30 | 云南大学 | A kind of difference element doping graphene quantum dot is respectively with molecular engram compound gas sensitive and the preparation method and application thereof |
| CN108732207B (en) * | 2018-04-17 | 2020-03-20 | 上海理工大学 | Sensitive material for formaldehyde detection and preparation method and application thereof |
| CN108693221B (en) * | 2018-04-18 | 2020-09-11 | 安徽工业大学 | Composite gas-sensitive material with high selectivity to low-concentration acetone |
| CN109133176B (en) * | 2018-07-31 | 2020-07-31 | 漯河医学高等专科学校 | ZnO-CeO2-WO3-Al2O3Preparation method of sensor material and acetone cyanohydrin gas sensor |
| CN109459470A (en) * | 2018-11-27 | 2019-03-12 | 中国石油大学(华东) | Palladium/cobaltosic oxide-the graphene film sensitive to extremely low concentration acetone under a kind of lower temperature |
| CN110736770B (en) * | 2019-10-16 | 2022-04-19 | 郑州大学 | N-GQDs modified 3DOM In2O3Composite material and preparation method and application thereof |
| CN112362702B (en) * | 2020-11-13 | 2023-06-27 | 安徽工业大学 | Composite gas-sensitive material with high gas-sensitive selectivity and low detection limit for toluene at room temperature |
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