CN104198540B - A kind of gas sensitive for detecting low concentration acetaldehyde - Google Patents
A kind of gas sensitive for detecting low concentration acetaldehyde Download PDFInfo
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- CN104198540B CN104198540B CN201410478950.5A CN201410478950A CN104198540B CN 104198540 B CN104198540 B CN 104198540B CN 201410478950 A CN201410478950 A CN 201410478950A CN 104198540 B CN104198540 B CN 104198540B
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Abstract
The invention discloses a kind of novel gas sensitive highly sensitive to aldehydes gas, belong to gas sensitive technical field.The present invention is with SnO2For base material, by solvent thermal reaction method (ethanol as solvent) at SnO2Middle incorporation Sb2O3And Graphene, wherein SnO2With Sb2O3Mol ratio be between 8 10, graphene-doped amount is SnO2And Sb2O3The 0.08 1.0% of quality sum.The heater-type gas sensor made as sensitive material using this material, under 25 DEG C of operating temperatures, to the sensitivity of 0.1ppm acetaldehyde (component resistance ratio in component resistance and tested gas in air) between 1.3 1.5, to the sensitivity of 1000ppm acetaldehyde between 60 70.
Description
Technical field
The invention belongs to gas sensitive, this material is used for making gas sensor, the gas sensor pair made
In air, low concentration acetaldehyde has high sensitivity and preferable selectivity.
Technical background
The general toxicity of acetaldehyde mainly shows as the direct stimulation to skin, eyes and upper respiratory tract mucosa,
Making expectorant increase, bloodshot eyes is red and swollen, causes allergy, headache etc..The acetaldehyde of suction high concentration then can cause and suffocate, even
Respiratory paralysis and dead.Acetaldehyde can form adduct with DNA covalent bond, cause between DNA crosslinking and
DNA breaks etc., acetaldehyde has an effect on the growth of embryo.Along with growth in the living standard and the enhancing of health consciousness,
People increasingly pay close attention to the existence of acetaldehyde.Accurately acetaldehyde in detection air, has the heaviest for protection health
The meaning wanted.
At present the method for acetaldehyde is mainly gas chromatography, spectrophotography, height in sensing chamber or in workshop air
Effect liquid phase chromatogram method and chemoluminescence method etc., these methods need more complicated, expensive instrument.Metal oxygen
Compound semiconductor gas sensor due to cheap, be prone to make, can be implemented in line detection and by wide
General attention.Yasuhiro Shimizu etc. (Journal of The Electrochemical Society,
146 (3) 1222-1226 (1999)) in tin ash, mix 0.1wt%Rh, material is made element and is existed
To the sensitivity of the sensitivity of 40ppm acetaldehyde (component resistance and tested gas in air under 350 DEG C of operating temperatures
Component resistance ratio in body) reach 2 times.(the Bull.Korean Chem.Soc. such as Jae-Mok Jun
32 (6) 1865-1872 (2011)) in WO3, mix 5wt%SnO2 and 1wt%Ru, make thick film
Element reaches 10 to 100ppm acetaldehyde sensitivity under 300 DEG C of operating temperatures.The metal of document report at present
Oxide semiconductor acetaldehyde sensitive material and the operating temperature of sensor thereof and detection limit are higher.
Summary of the invention
The technical problem to be solved is to provide a kind of quick for detecting the gas of acetaldehyde concentration in air
Sense material, to improving aldehydes gas sensor to the power of test of low concentration acetaldehyde, the work that reduces sensor
Make temperature and the minimum detectability to acetaldehyde.
The gas sensitive of the present invention is with SnO2For base material, existed by solvent thermal reaction method (ethanol as solvent)
SnO2Middle incorporation Sb2O3And Graphene, wherein SnO2With Sb2O3Mol ratio be between 8-10, mix
The amount of Graphene is SnO2And Sb2O3The 0.08-1.0% of quality sum.
Prepared by this material solvent-thermal method, i.e. according to certain mol proportion, butter of tin, Butter of antimony. are dissolved in second
In alcohol, being joined by a certain amount of Graphene in above-mentioned mixed solution, ultrasonic disperse 1 hour, then limit is stirred
Mix limit and be added dropwise over NaOH ethanol solution, the molal quantity of the NaOH butter of tin molal quantity and 3 equal to 4 times
Butter of antimony. molal quantity sum again, is transferred to mixture in the autoclave of band politef,
100-140 DEG C is incubated 8-24 hour, allows reactor naturally cool to room temperature, is filtered, uses deionized water by product
Can't check chloride ion with in washing with alcohol to filtrate, 60 DEG C of vacuum drying, i.e. obtain gas sensitive.
The material of the present invention can utilize this material to make other as the sensitive material of aldehydes gas sensing element
The method of hot type gas sensor is: 0.1 gram of material and 0.5 gram of terpineol mixed grinding are made slurry, with little
Slurry is coated onto the surface of alumina ceramic tube by hairbrush；The size of alumina ceramic tube is: long 6 millimeters, interior
1.6 millimeters of footpath, external diameter 2 millimeters, at alumina tube two ends, gold medal makees electrode, and electrode is welded with spun gold conduct
Lead-in wire, the spacing of electrode is 1 millimeter；In alumina tube, placement nichrome wire is as heater strip, logical
Cross the electric current controlling to flow through heater strip and heater strip both end voltage can control alumina tube surface-sensitive material
Temperature；The alumina tube scribbling sensitive material slurry is placed under infrared lamp drying, i.e. obtains heater-type air-sensitive
Element.Element is at the working temperature to the sensitivity of certain gas, and element resistance in atmosphere and element exist
The ratio of resistance in tested gas.Element reaches 0.1ppm to the minimum detectability of acetaldehyde, and normal to indoor
See that dusty gas 1000ppm acetaldehyde, 1000ppm ammonia, the sensitivity of 1000ppm benzene are below 3.
Detailed description of the invention
Below with specific embodiment illustrative material to the high sensitivity of acetaldehyde, low detection limit and good selectivity.
Embodiment 1
The Graphene alcohol suspension that 0.75ml concentration is 1mg/ml is joined ultrasonic disperse 1 in 30ml ethanol
Add the stirring of 1ml concentrated hydrochloric acid after hour, be separately added into 0.0005mol SbCl3With 0.0045mol SnCl4,
Continuing ultrasonic disperse 1 hour after stirring and dissolving, being added dropwise over 10ml concentration while stirring is 1.95mol/L's
The ethanol solution of NaOH, after stirring 10 minutes, it is 50ml band politef that mixture is transferred to volume
Autoclave in, 100 DEG C be incubated 10 hours, allow reactor naturally cool to room temperature, by product mistake
Filter, to filtrate, can't check chloride ion by deionized water and washing with alcohol, 60 DEG C of vacuum drying, i.e. obtain
(in material, the mol ratio of Sn/Sb is 9 to gas sensitive, and graphene-doped amount is SnO2And Sb2O3Quality
The 0.1% of sum).
Material is made heater-type element, record element under 20 DEG C of operating temperatures to 0.1ppm, 1ppm,
The sensitivity of 10ppm, 100ppm, 1000ppm acetaldehyde is respectively 1.4,2.0,5.1,10,65.And phase
With under operating temperature, the acetaldehyde of 1000ppm and the sensitivity of 100ppm benzene are only had 1.3 and 1.9.Right
The acetaldehyde response time of 0.1-1000pp and recovery time are all less than 30 seconds.
Embodiment 2
The Graphene alcohol suspension that 0.55ml concentration is 1mg/ml is joined ultrasonic disperse 1 in 30ml ethanol
Add the stirring of 1ml concentrated hydrochloric acid after hour, be separately added into 0.0005mol SbCl3With 0.004mol SnCl4, stir
Continue ultrasonic disperse 1 hour after mixing dissolving, be added dropwise over the NaOH that 10ml concentration is 1.75mol/L while stirring
Ethanol solution, after stirring 10 minutes, mixture is transferred to the height that volume is 50ml band politef
In pressure reactor, it is incubated 16 hours at 120 DEG C, allows reactor naturally cool to room temperature, product is filtered,
To filtrate, can't check chloride ion by deionized water and washing with alcohol, 60 DEG C of vacuum drying, i.e. obtain air-sensitive
(in material, the mol ratio of Sn/Sb is 8 to material, and graphene-doped amount is SnO2And Sb2O3Quality sum
0.08%).
Material is made heater-type element, record element under 20 DEG C of operating temperatures to 0.1ppm, 1ppm,
The sensitivity of 10ppm, 100ppm, 1000ppm acetaldehyde is respectively 1.3,1.9,5.0,9.0,60.And phase
With under operating temperature, the acetaldehyde of 1000ppm and the sensitivity of 100ppm benzene are only had 1.2 and 1.8.Right
The acetaldehyde response time of 0.1-1000pp and recovery time are all less than 35 seconds.
Embodiment 3
The Graphene alcohol suspension that 8.3ml concentration is 1mg/ml is joined ultrasonic disperse 1 in 22ml ethanol
Add the stirring of 1ml concentrated hydrochloric acid after hour, be separately added into 0.0005mol SbCl3With 0.005mol SnCl4, stir
Continue ultrasonic disperse 1 hour after mixing dissolving, be added dropwise over the NaOH that 10ml concentration is 2.15mol/L while stirring
Ethanol solution, after stirring 10 minutes, mixture is transferred to the height that volume is 50ml band politef
In pressure reactor, it is incubated 24 hours at 140 DEG C, allows reactor naturally cool to room temperature, product is filtered,
To filtrate, can't check chloride ion by deionized water and washing with alcohol, 60 DEG C of vacuum drying, i.e. obtain air-sensitive
(in material, the mol ratio of Sn/Sb is 10 to material, and graphene-doped amount is SnO2And Sb2O3Quality sum
1%).
Material is made heater-type element, record element under 20 DEG C of operating temperatures to 0.1ppm, 1ppm,
The sensitivity of 10ppm, 100ppm, 1000ppm acetaldehyde is respectively 1.5,2.2,5.8,11,70.And phase
With under operating temperature, the acetaldehyde of 1000ppm and the sensitivity of 100ppm benzene are only had 1.4 and 2.0.Right
The acetaldehyde response time of 0.1-1000pp and recovery time are all less than 40 seconds.
Claims (1)
1. the gas sensitive being used for detecting low concentration acetaldehyde, it is characterised in that this material is at SnO2
Middle doping Sb2O3With the composite of Graphene, wherein: the mol ratio of Sn Yu Sb is 8～10, Graphene
Quality be SnO2And Sb2O3The 0.08～1.0% of quality sum.
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| CN201410478950.5A CN104198540B (en) | 2014-09-18 | 2014-09-18 | A kind of gas sensitive for detecting low concentration acetaldehyde |
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| CN201410478950.5A CN104198540B (en) | 2014-09-18 | 2014-09-18 | A kind of gas sensitive for detecting low concentration acetaldehyde |
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| CN104198540B true CN104198540B (en) | 2016-08-24 |
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| CN106053549B (en) * | 2016-05-30 | 2019-02-19 | 安徽工业大学 | It is a kind of for detecting the gas sensitive of low concentration acetone |
| KR101840191B1 (en) * | 2016-11-02 | 2018-03-21 | 한국전력공사 | Device for acetylene gas analysis of underground transmission cables and method for acetylene gas analysis |
| CN108593718A (en) * | 2018-05-22 | 2018-09-28 | 广东美的制冷设备有限公司 | Gas sensor sensitive material and preparation method thereof |
| CN110455889A (en) * | 2019-08-14 | 2019-11-15 | 吉林大学 | Based on YSZ and NiTiO3Sensitive electrode blendes together electric potential type acetaldehyde sensor and preparation method thereof |
| CN113173602B (en) * | 2021-04-14 | 2023-10-13 | 扬州大学 | Preparation method of n-nonanal volatile gas sensitive material |
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| CN85100030A (en) * | 1985-04-01 | 1986-06-10 | 天津大学 | Thin film SnO 2 gas-sensitive element and manufacture method thereof |
| CN101140254B (en) * | 2007-10-16 | 2010-08-11 | 上海大学 | Method for enhancing air-sensitive performance of metal oxide semiconductor material |
| CN103995088B (en) * | 2014-05-26 | 2015-12-02 | 太原理工大学 | The preparation method of Graphene/tin oxide nano composite material and application thereof |
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