CN109001266B - Composite gas-sensitive material with high sensitivity and high selectivity to acetic acid gas - Google Patents
Composite gas-sensitive material with high sensitivity and high selectivity to acetic acid gas Download PDFInfo
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- CN109001266B CN109001266B CN201811051058.3A CN201811051058A CN109001266B CN 109001266 B CN109001266 B CN 109001266B CN 201811051058 A CN201811051058 A CN 201811051058A CN 109001266 B CN109001266 B CN 109001266B
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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
Abstract
The invention discloses aA composite gas-sensitive material with high sensitivity and high selectivity to acetic acid gas belongs to the technical field of gas-sensitive materials. The composite gas-sensitive material consists of C3N4‑SnO2In which C is3N4The mass of (A) is 8-12% of the total mass of the material. The sensitivity of the indirectly heated gas-sensitive sensor made of the material as a sensitive material to 0.1ppm acetic acid is between 1.1 and 1.3 at 185 ℃, the sensitivity of the element to 1000ppm acetic acid reaches 35 to 90, and the sensitivity to 1000ppm acetone, formaldehyde, ethanol, acetaldehyde and ammonia gas is below 8, which shows that C is C3N4The sensitivity and gas sensitivity selectivity of tin dioxide to acetic acid gas are improved, the working temperature of the acetic acid gas sensor is reduced, the concentration of acetic acid in air can be rapidly detected, and the interference of acetone, formaldehyde, ethanol, acetaldehyde, ammonia gas and other gases is eliminated.
Description
Technical Field
The invention belongs to the technical field of gas-sensitive materials, and particularly relates to a composite gas-sensitive material which is used for manufacturing a gas sensor.
Background
Acetic acid is a volatile colorless liquid with strong pungent odor, has strong corrosivity, can cause skin and mucosa blister, red swelling symptom, and causes rhinitis, bronchitis when the concentration is high, and acute chemical pneumonia can occur in serious cases. The sanitary standard in America, Japan and the like is 25mg/m3(about 9.3ppm), the limit of acetic acid in air of a working place is not established in China. The existing methods for measuring the concentration of acetic acid in air mainly adopt gas chromatography, ion chromatography and the like, and the methods need expensive instruments and equipment, and take a long time for sampling analysis.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a high-sensitivity and high-selectivity gas sensitive material for detecting acetic acid gas in air at a lower working temperature, so that the material can eliminate the interference of acetone, formaldehyde, ethanol, acetaldehyde, ammonia gas and the like on the detection of the acetic acid gas and realize the rapid detection of the concentration of the acetic acid gas in the air.
The invention is realized by the following technical scheme.
The invention provides a composite gas-sensitive material, which is formed by SnO2And C3N4Wherein: c3N4The mass of (A) accounts for 8-12% of the total mass of the material; the gas-sensitive material is prepared by the following steps:
(1)C3N4preparation: 2 g of melamine were placed in a crucible, raised to 520 ℃ in a muffle furnace at a rate of 5 ℃/min and kept at a constant temperature of 520 ℃ for 5 hours. After naturally cooling to room temperature, the product is washed with deionized water and absolute ethyl alcohol for three times respectively, dried for 24 hours at 60 ℃ and ground into powder for later use.
(2)SnO2Preparation: weighing a certain amount of SnCl4·5H2O, adding 20ml of water into a beaker, stirring for half an hour, and adjusting the pH value of the solution to 2 by using 2mol/L ammonia water solution. Transferring the reaction solution into a 100ml hydrothermal reaction kettle, reacting for 10 hours at 180 ℃, washing the obtained precipitate with absolute ethyl alcohol for three times, and drying the product at 80 ℃ for 24 hours to obtain SnO2。
(3)C3N4-SnO2Preparing a composite gas-sensitive material: weighing a certain amount of g-C3N4(g-C3N4Accounting for 8-12 wt% of the composite material), adding into 80ml of methanol, and ultrasonically dispersing for 1 hour to obtain g-C3N4And (3) suspension. Adding SnO into the suspension while stirring2And stirring in a fume hood for 12 hours until the methanol is completely volatilized, and drying the obtained precipitate in an oven at 80 ℃ for 24 hours to obtain the composite gas-sensitive material.
Furthermore, the composite gas sensitive material has poor sensitivity to acetone, formaldehyde, ethanol, acetaldehyde and ammonia gas.
The composite material can be used as a sensitive material of an acetic acid gas sensor, and the method for manufacturing the indirectly heated gas sensitive element by using the material comprises the following steps: mixing and grinding 0.1 g of the material and 0.5 g of terpineol to prepare slurry, and coating the slurry on the surface of an alumina ceramic tube by using a small brush; the dimensions of the alumina ceramic tube are: the length is 6 mm, the inner diameter is 1.6 mm, the outer diameter is 2 mm, gold prizes are used as electrodes at two ends of the alumina tube, gold wires are welded on the electrodes as leads, and the distance between the electrodes is 1 mm; placing a nickel-chromium alloy wire as a heating wire in the alumina tube, and controlling the temperature of the sensitive material on the surface of the alumina tube by controlling the current flowing through the heating wire and the voltage at two ends of the heating wire; and (3) drying the alumina tube coated with the sensitive material slurry under an infrared lamp to obtain the indirectly heated gas sensitive element. The sensitivity of the element to a gas is the ratio of the resistance of the element in air to the resistance of the element in the gas being measured at the operating temperature.
Compared with the prior art, the invention has the following technical effects:
1. the invention mixes C into tin dioxide by a hydrothermal reaction method3N4The optimum working temperature of the gas sensor made of the material for detecting acetic acid gas is 185 ℃, which is lower than the optimum working temperature (235 ℃) of the gas sensor made of pure tin dioxide material.
2. At 185 deg.C, the sensitivity to 0.1ppm acetic acid (the ratio of the resistance of the element in air to the resistance of the element in the gas to be measured) is 1.1-1.3, the sensitivity to 1000ppm acetic acid is 35-90, but the sensitivity to acetone, formaldehyde, ethanol, acetaldehyde and ammonia gas with the same concentration is below 8, so that the interference of acetone, formaldehyde, ethanol, acetaldehyde and ammonia gas can be eliminated, which shows that C is a reference3N4The sensitivity and selectivity of tin dioxide to acetic acid gas are improved.
3. The material has short response recovery time to acetic acid gas (for example, the response and recovery time to 0.1ppm acetic acid gas do not exceed 18s), and can realize the rapid detection of the concentration of acetic acid in the air.
Detailed Description
The present invention will be described in detail with reference to specific examples, but the present invention is not limited to the examples.
Example 1
Weighing 0.0080g of g-C3N4(g-C3N4Accounting for 8wt percent of the composite material), adding into 80ml of methanol, and carrying out ultrasonic dispersion for 1 hour to obtain g-C3N4And (3) suspension. 0.0920g SnO was added to the suspension while stirring2And stirring in a fume hood for 12 hours until the methanol is completely volatilized, and drying the obtained precipitate in an oven at 80 ℃ for 24 hours to obtain the composite material.
The material is made into an indirectly heated element, and the highest sensitivity of the indirectly heated element to 0.1, 1, 10, 100 and 1000ppm acetic acid gas at 185 ℃ is respectively 1.1, 1.5, 4.2, 6.8, 11.4 and 35.0; the sensitivity to 1000ppm acetone, formaldehyde, ethanol, acetaldehyde and ammonia gas is below 3.5; response time and recovery time for 0.1ppm acetic acid did not exceed 16 seconds.
Example 2
Weighing 0.0100g of g-C3N4(g-C3N4Accounting for 10wt percent of the composite material), adding into 80ml of methanol, and carrying out ultrasonic dispersion for 1 hour to obtain g-C3N4And (3) suspension. 0.0900g SnO was added to the suspension with stirring2And stirring in a fume hood for 12 hours until the methanol is completely volatilized, and drying the obtained precipitate in an oven at 80 ℃ for 24 hours to obtain the composite material.
The material is made into an indirectly heated element, and the highest sensitivity of the indirectly heated element to 0.1, 1, 10, 100 and 1000ppm acetic acid gas at 185 ℃ is respectively 1.2, 1.6, 4.8, 12.4, 28.3 and 88.5; the sensitivity to 1000ppm acetone, formaldehyde, ethanol, acetaldehyde and ammonia gas is below 8; response time and recovery time for 0.1ppm acetic acid did not exceed 15 seconds.
Example 3
Weighing 0.0110g of g-C3N4(g-C3N411 wt% of the composite material), adding 80ml of methanol, and performing ultrasonic dispersion for 1 hour to obtain g-C3N4And (3) suspension. 0.0890g SnO was added to the suspension with stirring2And stirring in a fume hood for 12 hours until the methanol is completely volatilized, and drying the obtained precipitate in an oven at 80 ℃ for 24 hours to obtain the composite material.
The material is made into an indirectly heated element, and the highest sensitivity of the indirectly heated element to 0.1, 1, 10, 100 and 1000ppm acetic acid gas at 185 ℃ is respectively 1.3, 1.8, 4.6, 10.1, 22.2 and 40.2; the sensitivity to 1000ppm acetone, formaldehyde, ethanol, acetaldehyde and ammonia gas is below 3.5; response time and recovery time for 0.1ppm acetic acid did not exceed 18 seconds.
Example 4
Weighing 0.0120g of g-C3N4(g-C3N411 wt% of the composite material), adding 80ml of methanol, and performing ultrasonic dispersion for 1 hour to obtain g-C3N4And (3) suspension. 0.0880g SnO was added to the suspension while stirring2And stirring in a fume hood for 12 hours until the methanol is completely volatilized, and drying the obtained precipitate in an oven at 80 ℃ for 24 hours to obtain the composite material.
The material is made into an indirectly heated element, and the highest sensitivity of the indirectly heated element to 0.1, 1, 10, 100 and 1000ppm acetic acid gas at 185 ℃ is respectively 1.2, 1.7, 4.1, 8.9, 17.6 and 38.4; the sensitivity to 1000ppm acetone, formaldehyde, ethanol, acetaldehyde and ammonia gas is below 4; response time and recovery time for 0.1ppm acetic acid did not exceed 16 seconds.
Claims (2)
1. A composite gas-sensitive material with high sensitivity and selectivity to acetic acid gas is characterized in that the gas-sensitive material consists of SnO2And C3N4Wherein: c3N4The mass of (A) accounts for 8-12% of the total mass of the material; the gas sensitive material has poor sensitivity to acetone, formaldehyde, ethanol, acetaldehyde and ammonia gas; the gas-sensitive material is prepared by the following steps:
(1)C3N4the preparation of (1): melamine was placed in a crucible, raised to 520 ℃ in a muffle furnace at a rate of 5 ℃/min and held at 520 ℃ for 5 hours; naturally cooling to room temperature, washing the product with deionized water and absolute ethyl alcohol respectively, drying at 60 ℃ for 24 hours, and grinding into powder for later use;
(2)SnO2the preparation of (1): weighing SnCl4·5H2Adding 20ml of water into a beaker, stirring for half an hour, and adjusting the pH value of the solution to 2 by using 2mol/L ammonia water solution; will be reversedTransferring the reaction solution into a 100ml hydrothermal reaction kettle, reacting for 10 hours at 180 ℃, washing the obtained precipitate with absolute ethyl alcohol, and drying the product at 80 ℃ for 24 hours to obtain SnO2；
(3) Preparing a composite gas-sensitive material: weighing C prepared in step (1)3N4Adding into 80ml of methanol, and ultrasonically dispersing for 1 hour to obtain g-C3N4A suspension; adding the SnO prepared in the step (2) into the suspension while stirring2Stirring in a fume hood for 12 hr until methanol is completely volatilized, oven drying the obtained precipitate at 80 deg.C for 24 hr to obtain C3N4-SnO2A composite gas sensitive material.
2. Use of a gas sensor made of the composite gas-sensitive material according to claim 1 for detecting acetic acid gas.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109682867B (en) * | 2019-01-23 | 2022-05-24 | 陕西科技大学 | Micron-sized tin dioxide gas-sensitive material and preparation method and application thereof |
| CN110095510B (en) * | 2019-05-28 | 2020-11-06 | 安徽工业大学 | Sm-doped NiGa with high sensitivity and high selectivity on methanol gas2O4Composite material |
| CN110133058B (en) * | 2019-05-28 | 2020-10-16 | 安徽工业大学 | La-doped NiGa with high gas sensitivity selectivity to acetic acid gas2O4Nanocomposite material |
| CN110095513B (en) * | 2019-05-30 | 2021-01-01 | 安徽工业大学 | g-C with high gas sensitivity selectivity to trimethylamine gas3N4-ZnGa2O4Nanocomposite material |
| CN110841682B (en) * | 2019-11-09 | 2022-09-02 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of tin oxide modified graphite-like phase carbon nitride nanosheet, product 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 |
| CN113219011B (en) * | 2021-05-19 | 2022-08-09 | 吉林大学 | Co-doped SnO 2 Formaldehyde-acetone gas sensor and preparation method thereof |
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| CN105688944A (en) * | 2016-03-14 | 2016-06-22 | 西安建筑科技大学 | Method for preparing layered MoS2-SnO2 nano composite material |
| CN106995673A (en) * | 2017-04-14 | 2017-08-01 | 广东工业大学 | A kind of low-gravity composite heat-conducting insulating cement and preparation method thereof |
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| CN105688944A (en) * | 2016-03-14 | 2016-06-22 | 西安建筑科技大学 | Method for preparing layered MoS2-SnO2 nano composite material |
| CN106995673A (en) * | 2017-04-14 | 2017-08-01 | 广东工业大学 | A kind of low-gravity composite heat-conducting insulating cement and preparation method thereof |
| CN107192743A (en) * | 2017-06-15 | 2017-09-22 | 哈尔滨工业大学 | A kind of preparation method of flower-shaped graded structure stannic disulfide/stannic oxide nanometer composite air-sensitive material |
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