CN104198540A - Gas sensitive material for detecting low-concentration acetaldehyde - Google Patents
Gas sensitive material for detecting low-concentration acetaldehyde Download PDFInfo
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- CN104198540A CN104198540A CN201410478950.5A CN201410478950A CN104198540A CN 104198540 A CN104198540 A CN 104198540A CN 201410478950 A CN201410478950 A CN 201410478950A CN 104198540 A CN104198540 A CN 104198540A
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- acetaldehyde
- gas sensitive
- sensitive material
- sensitivity
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Abstract
The invention discloses a novel gas sensitive material for detecting the high sensitivity of acetaldehyde gas and belongs to the technical field of gas sensitive materials. The novel gas sensitive material takes SnO2 as a basic material and is characterized in that Sb2O3 and grapheme are mixed in the SnO2 through a solvent thermal reaction method (ethanol is taken as a solvent), wherein the molar ratio of the SnO2 to the Sb2O3 ranges from 8 to 10, and the amount of the mixed grapheme is 0.08-1.0 percent of the sum of the mass of the SnO2 and the Sb2O3. The novel gas sensitive material has the benefits that the sensitivity of an indirectly heated type gas sensitive sensor made of the gas sensitive material to the acetaldehyde of 0.1 ppm (ratio of element resistance in air to element resistance in measured gas) at a working temperature of 25 DEG C ranges from 1.3 to 1.5, and the sensitivity to the acetaldehyde of 1000 mmp ranges from 60 and 70.
Description
Technical field
The invention belongs to gas sensitive, this material is used for making gas sensor, and the gas sensor of making has high sensitivity and better selectivity to low concentration acetaldehyde in air.
Technical background
The general toxicity main manifestations of acetaldehyde is the direct spread effect to skin, eyes and upper respiratory tract mucosa, and phlegm is increased, and bloodshot eyes redness, causes allergy, headache etc.Suck the acetaldehyde of high concentration and can cause and suffocate, even respiratory paralysis and death.Acetaldehyde can form adduct with DNA covalent bond, causes DNA interchain linkage and DNA break etc., and acetaldehyde also affects embryo's growth.Along with the enhancing of growth in the living standard and health consciousness, people more and more pay close attention to the existence of acetaldehyde.Accurately detect acetaldehyde in air, be of great significance for protection health.
At present the method for acetaldehyde is mainly vapor-phase chromatography, spectrophotometric method, high performance liquid chromatography and chemoluminescence method etc. in sensing chamber or in workshop air, and these methods need the instrument of more complicated, costliness.Metal Oxide Semiconductor Gas Sensing sensor due to cheap, be easy to make, can realize online detection and in widespread attention.(the Journal of The Electrochemical Society such as Yasuhiro Shimizu, 146 (3) 1222-1226 (1999)) in tin ash, mix 0.1wt%Rh, the sensitivity (in air in component resistance and tested gas component resistance ratio) that material is made element sensitivity to 40ppm acetaldehyde under 350 DEG C of working temperatures reaches 2 times.Jae-Mok Jun etc. (Bull.Korean Chem.Soc.32 (6) 1865-1872 (2011)) mix 5wt%SnO2 and 1wt%Ru in WO3, and to 100ppm acetaldehyde, sensitivity reaches 10 under 300 DEG C of working temperatures to make thick film element.The metal-oxide semiconductor (MOS) acetaldehyde sensitive material of bibliographical information and working temperature and the detection limit of sensor are higher at present.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of gas sensitive material for detection of acetaldehyde concentration in air, to improving detectability, the working temperature that reduce sensor and the minimum detectability to acetaldehyde of aldehydes gas sensor to low concentration acetaldehyde.
Gas sensitive of the present invention is with SnO
2for base-material, by solvent thermal reaction method (ethanol is made solvent) at SnO
2in mix Sb
2o
3and Graphene, wherein SnO
2with Sb
2o
3mol ratio be between 8-10, graphene-doped amount is SnO
2and Sb
2o
3the 0.08-1.0% of quality sum.
This material is prepared with solvent-thermal method, according to certain mol proportion by butter of tin, antimony trichloride is dissolved in ethanol, a certain amount of Graphene is joined in above-mentioned mixed solution, ultrasonic dispersion 1 hour, then dropwise add while stirring NaOH ethanolic solution, the molal quantity of NaOH equals the butter of tin molal quantity of 4 times and the antimony trichloride molal quantity sum of 3 times, potpourri is transferred in the autoclave with teflon, at 100-140 DEG C of insulation 8-24 hour, allow reactor naturally cool to room temperature, product is filtered, wash to filtrate and can't check chlorion with deionized water and ethanol, 60 DEG C of vacuum drying, obtain gas sensitive.
Material of the present invention can be used as the sensitive material of aldehydes gas sensitive element, the method of utilizing this material to make heater-type gas sensor is: 0.1 gram of material and 0.5 gram of terpinol mixed grinding are made to slurry, with small brushes, slurry is coated onto to the surface of alumina ceramic tube; The size of alumina ceramic tube is: long 6 millimeters, and 1.6 millimeters of internal diameters, 2 millimeters of external diameters, make electrode at alumina tube two ends with gold medal, are welded with spun gold as lead-in wire on electrode, and between electrode, distance is 1 millimeter; In alumina tube, place nichrome wire as heater strip, flow through the electric current of heater strip and heater strip both end voltage and can control the temperature of alumina tube surface-sensitive material by control; The alumina tube that scribbles sensitive material slurry is placed under infrared lamp and is dried, obtain heater-type gas sensor.Element is under working temperature to the sensitivity of certain gas, the ratio of element resistance and element resistance in tested gas in air.Element reaches 0.1ppm to the minimum detectability of acetaldehyde, and to the sensitivity of indoor common dusty gas 1000ppm acetaldehyde, 1000ppm ammonia, 1000ppm benzene all lower than 3.
Embodiment
The high sensitivity to acetaldehyde, low detection limit and good selectivity with specific embodiment illustrative material below.
Embodiment 1
The Graphene alcohol suspension that is 1mg/ml by 0.75ml concentration joins ultrasonic dispersion in 30ml ethanol and after 1 hour, adds 1ml concentrated hydrochloric acid to stir, and adds respectively 0.0005mol SbCl
3with 0.0045mol SnCl
4after stirring and dissolving, continue ultrasonic dispersion 1 hour, dropwise adding while stirring 10ml concentration is the ethanolic solution of the NaOH of 1.95mol/L, stir after 10 minutes, it is in the autoclave of 50ml with teflon that potpourri is transferred to volume, 100 DEG C of insulations 10 hours, allow reactor naturally cool to room temperature, product is filtered, washs to filtrate and can't check chlorion with deionized water and ethanol, 60 DEG C of vacuum drying, (in material, the mol ratio of Sn/Sb is 9, and graphene-doped amount is SnO to obtain gas sensitive
2and Sb
2o
3quality sum 0.1%).
Material is made to heater-type element, record element, under 20 DEG C of working temperatures, the sensitivity of 0.1ppm, 1ppm, 10ppm, 100ppm, 1000ppm acetaldehyde is respectively to 1.4,2.0,5.1,10,65.And under identical working temperature, the sensitivity of the acetaldehyde to 1000ppm and 100ppm benzene only has 1.3 and 1.9.Acetaldehyde response time and release time to 0.1-1000pp are all no more than 30 seconds.
Embodiment 2
The Graphene alcohol suspension that is 1mg/ml by 0.55ml concentration joins ultrasonic dispersion in 30ml ethanol and after 1 hour, adds 1ml concentrated hydrochloric acid to stir, and adds respectively 0.0005mol SbCl
3with 0.004mol SnCl
4after stirring and dissolving, continue ultrasonic dispersion 1 hour, dropwise adding while stirring 10ml concentration is the ethanolic solution of the NaOH of 1.75mol/L, stir after 10 minutes, it is in the autoclave of 50ml with teflon that potpourri is transferred to volume, 120 DEG C of insulations 16 hours, allow reactor naturally cool to room temperature, product is filtered, washs to filtrate and can't check chlorion with deionized water and ethanol, 60 DEG C of vacuum drying, (in material, the mol ratio of Sn/Sb is 8, and graphene-doped amount is SnO to obtain gas sensitive
2and Sb
2o
3quality sum 0.08%).
Material is made to heater-type element, record element, under 20 DEG C of working temperatures, the sensitivity of 0.1ppm, 1ppm, 10ppm, 100ppm, 1000ppm acetaldehyde is respectively to 1.3,1.9,5.0,9.0,60.And under identical working temperature, the sensitivity of the acetaldehyde to 1000ppm and 100ppm benzene only has 1.2 and 1.8.Acetaldehyde response time and release time to 0.1-1000pp are all no more than 35 seconds.
Embodiment 3
The Graphene alcohol suspension that is 1mg/ml by 8.3ml concentration joins ultrasonic dispersion in 22ml ethanol and after 1 hour, adds 1ml concentrated hydrochloric acid to stir, and adds respectively 0.0005mol SbCl
3with 0.005mol SnCl
4after stirring and dissolving, continue ultrasonic dispersion 1 hour, dropwise adding while stirring 10ml concentration is the ethanolic solution of the NaOH of 2.15mol/L, stir after 10 minutes, it is in the autoclave of 50ml with teflon that potpourri is transferred to volume, 140 DEG C of insulations 24 hours, allow reactor naturally cool to room temperature, product is filtered, washs to filtrate and can't check chlorion with deionized water and ethanol, 60 DEG C of vacuum drying, (in material, the mol ratio of Sn/Sb is 10, and graphene-doped amount is SnO to obtain gas sensitive
2and Sb
2o
3quality sum 1%).
Material is made to heater-type element, record element, under 20 DEG C of working temperatures, the sensitivity of 0.1ppm, 1ppm, 10ppm, 100ppm, 1000ppm acetaldehyde is respectively to 1.5,2.2,5.8,11,70.And under identical working temperature, the sensitivity of the acetaldehyde to 1000ppm and 100ppm benzene only has 1.4 and 2.0.Acetaldehyde response time and release time to 0.1-1000pp are all no more than 40 seconds.
Claims (1)
1. for detection of a gas sensitive for low concentration acetaldehyde, it is characterized in that, this material is at SnO
2middle doping Sb
2o
3with the compound substance of Graphene, wherein: the mol ratio of Sn and Sb is 8～10, the quality of Graphene is SnO
2and Sb
2o
30.08～1.0% of quality sum.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| CN104198540A true CN104198540A (en) | 2014-12-10 |
| CN104198540B CN104198540B (en) | 2016-08-24 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106053549A (en) * | 2016-05-30 | 2016-10-26 | 安徽工业大学 | Gas sensitive material for detecting low-concentration acetone |
| 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 |
| CN109716118A (en) * | 2016-11-02 | 2019-05-03 | 韩国电力公社 | Acetylene gas analytical equipment and analysis method for buried cable |
| 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 |
| CN113173602A (en) * | 2021-04-14 | 2021-07-27 | 扬州大学 | Preparation method of n-nonanal volatile gas sensitive material |
Citations (3)
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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 |
| CN101140254A (en) * | 2007-10-16 | 2008-03-12 | 上海大学 | Method for enhancing air-sensitive performance of metal oxide semiconductor material |
| CN103995088A (en) * | 2014-05-26 | 2014-08-20 | 太原理工大学 | Preparation method and application of graphene/tin oxide nano composite material |
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2014
- 2014-09-18 CN CN201410478950.5A patent/CN104198540B/en active Active
Patent Citations (3)
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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 |
| CN101140254A (en) * | 2007-10-16 | 2008-03-12 | 上海大学 | Method for enhancing air-sensitive performance of metal oxide semiconductor material |
| CN103995088A (en) * | 2014-05-26 | 2014-08-20 | 太原理工大学 | Preparation method and application of graphene/tin oxide nano composite material |
Non-Patent Citations (1)
| Title |
|---|
| 高晓平等: "基于锑掺杂的高灵敏度纳米SnO2气体传感器", 《仪表技术与传感器》, 31 December 2009 (2009-12-31) * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106053549A (en) * | 2016-05-30 | 2016-10-26 | 安徽工业大学 | Gas sensitive material for detecting low-concentration acetone |
| 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 |
| CN109716118A (en) * | 2016-11-02 | 2019-05-03 | 韩国电力公社 | Acetylene gas analytical equipment and analysis method for buried cable |
| 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 |
| CN113173602A (en) * | 2021-04-14 | 2021-07-27 | 扬州大学 | Preparation method of n-nonanal volatile gas sensitive material |
| CN113173602B (en) * | 2021-04-14 | 2023-10-13 | 扬州大学 | Preparation method of n-nonanal volatile gas sensitive material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104198540B (en) | 2016-08-24 |
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