CN108693221B - Composite gas-sensitive material with high selectivity to low-concentration acetone - Google Patents
Composite gas-sensitive material with high selectivity to low-concentration acetone Download PDFInfo
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- CN108693221B CN108693221B CN201810349324.4A CN201810349324A CN108693221B CN 108693221 B CN108693221 B CN 108693221B CN 201810349324 A CN201810349324 A CN 201810349324A CN 108693221 B CN108693221 B CN 108693221B
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Abstract
The invention discloses a composite gas-sensitive material with high selectivity to low-concentration acetone, and belongs to the technical field of gas-sensitive materials. The gas sensitive material consists of graphene quantum dots-La2O3‑ZnFe2O4Composite material in which the mass of graphene quantum dots accounts for0.5-1.5% of the total mass of the material, La2O3And ZnFe2O4The molar ratio of (A) is 2.5-4%. The indirectly heated gas-sensitive sensor made of the material as a sensitive material has high gas-sensitive selectivity to acetone, when the working temperature is 125 ℃, the sensitivity of the element to 1000ppm acetone reaches 124-156, the sensitivity to 0.01ppm acetone gas reaches 1.5-2.2, and the response and recovery time to 0.01-1000ppm acetone gas respectively do not exceed 25s and 54 s; the gas sensor has very low sensitivity to common interference gas at 125 ℃, the sensitivity to 1000ppm ethanol, methanol, acetaldehyde and formaldehyde is not more than 14, and the sensitivity to 1000ppm ammonia, benzene, toluene and hydrogen is not more than 4.
Description
Technical Field
The invention belongs to the technical field of gas-sensitive materials, and particularly relates to a composite gas-sensitive material for detecting low-concentration acetone.
Background
Acetone is a common VOC gas, and has inhibitory and anesthetic effects on the central nervous system. The damage of acetone vapor to human body is mainly manifested by eye irritation such as lacrimation, photophobia and corneal epithelium infiltration, and also caused by vertigo, burning sensation, throat irritation, cough, etc. Therefore, the detection and monitoring of the acetone concentration in the ambient air are of great significance. In addition, acetone is a fat metabolite in a human body, the concentration of acetone in the exhaled air of a healthy person is lower than 0.9ppm, and the concentration of acetone exhaled by a diabetic patient is higher than 1.8ppm, so that quantitative analysis is helpful for the diagnosis of diabetes. The metal oxide gas sensitive material has high sensitivity to gas, but has the defects of low selectivity and interference by other gases.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a composite gas-sensitive material with high selectivity on low-concentration acetone.
The invention is realized by the following technical scheme.
The invention provides a composite gas-sensitive material with high selectivity to low-concentration acetone, which comprises graphene quantum dots and La2O3And ZnFe2O4Wherein: the graphene quantum dots account for 0.5-1.5% of the total mass of the material, and the La2O3And ZnFe2O4The molar ratio of (A) is 2.5-4%.
The invention also provides a preparation method of the composite gas-sensitive material with high selectivity to low-concentration acetone, which comprises the following steps:
(1) 0.001mol Zn (NO) is weighed3)2·6H2O、0.002molFe(NO3)3·9H2O、0.00005～0.00008molLa(NO3)3·6H2Dissolving O in 20mL of deionized water; slowly adding 1.5-4.5 ml of graphene quantum dot solution with the concentration of 1mg/g into the solution, stirring for 30min, and carrying out ultrasonic treatment on the mixed solution for 30min to obtain a suspension;
(2) dropwise adding 1mol/L NaOH solution into the suspension obtained in the step (1) until the pH value of the reaction solution is 7.0; adding deionized water to the volume of 70mL, transferring the reaction solution to a hydrothermal kettle with the volume of 100mL, reacting for 24 hours at 180-200 ℃, after the reaction kettle is cooled, washing the product with deionized water and absolute ethyl alcohol, and drying the washed precipitate in a drying oven at 60 ℃ for 24 hours to obtain the graphene quantum dot-La2O3-ZnFe2O4A composite gas sensitive material.
The material of the invention can be used as a sensitive material of an acetone gas sensitive element, and the method for manufacturing the indirectly heated gas sensitive element by utilizing 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:
the invention passes through waterThermal reaction method on ZnFe2O4Doped with graphene quantum dots and-La2O3The indirectly heated gas-sensitive sensor is prepared by taking the material as a sensitive material, and the gas-sensitive material has higher sensitivity to acetone at lower temperature, more importantly, has low sensitivity to other gases at the temperature and shows high gas-sensitive selectivity to acetone. When the working temperature is 125 ℃, the sensitivity of the element to 1000ppm acetone reaches 124-156, the sensitivity to common interference gas is very low, the sensitivity to 1000ppm ethanol, methanol, acetaldehyde and formaldehyde is respectively 9.8, 7.9, 8.8 and 12.3, and the sensitivity to 1000ppm ammonia, benzene, toluene and hydrogen is not more than 4.
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
0.001mol Zn (NO) is weighed3)2·6H2O、0.002molFe(NO3)3·9H2O and 0.00005mol La (NO)3)3·6H2Dissolving O in 20mL of deionized water, slowly adding 1.5mL of graphene quantum dot solution with the concentration of 1mg/g into the solution, stirring for 30min, and carrying out ultrasonic treatment on the mixed solution for 30min to obtain a suspension. Then, a 1mol/L NaOH solution was added dropwise to the suspension until the pH of the reaction solution became 7.0. Adding deionized water to the volume of 70mL, then transferring the reaction solution to a hydrothermal kettle with the volume of 100mL, reacting for 24h at 180 ℃, after the reaction kettle is cooled, washing the product for multiple times by using the deionized water and absolute ethyl alcohol, and putting the washed precipitate into an oven to be dried for 24h at the temperature of 60 ℃. Obtaining the graphene quantum dot-La2O3-ZnFe2O4A composite material. The material is analyzed by a thermogravimetric analysis method, and the content of the graphene quantum dots in the composite material is 0.5 wt%.
The material is made into an indirectly heated element, and the sensitivity of the indirectly heated element to 0.01, 0.1, 1, 10, 100 and 1000ppm acetone gas at the working temperature of 125 ℃ is measured to be 1.8, 3.4, 8.1, 22.6, 58.5 and 124.0 respectively. The response time and recovery time for 0.01-1000pp acetone do not exceed 22 seconds and 45 seconds. The sensitivity to 1000ppm ethanol, methanol, acetaldehyde and formaldehyde is respectively 9.0, 7.9, 8.8 and 12.3, and the sensitivity to 1000ppm ammonia, benzene, toluene and hydrogen is not more than 4.
Example 2
0.001mol Zn (NO) is weighed3)2·6H2O、0.002molFe(NO3)3·9H2O and 0.00008mol La (NO)3)3·6H2Dissolving O in 20mL of deionized water, slowly adding 4.5mL of graphene quantum dot solution with the concentration of 1mg/g into the solution, stirring for 30min, and carrying out ultrasonic treatment on the mixed solution for 30min to obtain a suspension. Then, a 1mol/L NaOH solution was added dropwise to the suspension until the pH of the reaction solution became 7.0. Adding deionized water to the volume of 70mL, then transferring the reaction solution to a hydrothermal kettle with the volume of 100mL, reacting for 24h at 200 ℃, after the reaction kettle is cooled, washing the product for multiple times by using the deionized water and absolute ethyl alcohol, and putting the washed precipitate into an oven to be dried for 24h at the temperature of 60 ℃. Obtaining the graphene quantum dot-La2O3-ZnFe2O4A composite material. The material is analyzed by a thermogravimetric analysis method, and the content of the graphene quantum dots in the composite material is 1.5 wt%.
The material is made into an indirectly heated element, and the sensitivity of the indirectly heated element to 0.01, 0.1, 1, 10, 100 and 1000ppm acetone gas at the working temperature of 125 ℃ is measured to be 2.0, 3.7, 8.9, 26.6, 70.6 and 156.0 respectively. The response time and recovery time for 0.01-1000pp acetone do not exceed 25 seconds and 54 seconds. The sensitivity to 1000ppm ethanol, methanol, acetaldehyde and formaldehyde is respectively 9.4, 8.9, 9.8 and 13.9, and the sensitivity to 1000ppm ammonia, benzene, toluene and hydrogen is not more than 4.
Example 3
0.001mol Zn (NO) is weighed3)2·6H2O、0.002molFe(NO3)3·9H2O and 0.00006mol La (NO)3)3·6H2Dissolving O in 20mL of deionized water, slowly adding 3.0mL of graphene quantum dot solution with the concentration of 1mg/g into the solution, stirring for 30min, and carrying out ultrasonic treatment on the mixed solution for 30min to obtain a suspension. Then adding 1mol/L NaOH solution into the suspensionThe pH of the reaction mixture was 7.0. Adding deionized water to the volume of 70mL, then transferring the reaction solution to a hydrothermal kettle with the volume of 100mL, reacting for 24h at 190 ℃, after the reaction kettle is cooled, washing the product for multiple times by using the deionized water and absolute ethyl alcohol, and putting the washed precipitate into an oven to be dried for 24h at the temperature of 60 ℃. Obtaining the graphene quantum dot-La2O3-ZnFe2O4A composite material. The material is analyzed by a thermogravimetric analysis method, and the content of the graphene quantum dots in the composite material is 1.0 wt%.
The material is made into an indirectly heated element, and the sensitivity of the indirectly heated element to 0.01, 0.1, 1, 10, 100 and 1000ppm acetone gas at the working temperature of 125 ℃ is measured to be 2.2, 3.4, 9.9, 28.8, 68.3 and 146.8 respectively. The response time and recovery time for 0.01-1000pp acetone do not exceed 20 seconds and 49 seconds. The sensitivity to 1000ppm ethanol, methanol, acetaldehyde and formaldehyde is respectively 9.9, 10.8, 11.8 and 12.9, and the sensitivity to 1000ppm ammonia, benzene, toluene and hydrogen is not more than 4.
Example 4
0.001mol Zn (NO) is weighed3)2·6H2O、0.002molFe(NO3)3·9H2O and 0.00006mol La (NO)3)3·6H2Dissolving O in 20mL of deionized water, slowly adding 4.0mL of graphene quantum dot solution with the concentration of 1mg/g into the solution, stirring for 30min, and carrying out ultrasonic treatment on the mixed solution for 30min to obtain a suspension. Then, a 1mol/L NaOH solution was added dropwise to the suspension until the pH of the reaction solution became 7.0. Adding deionized water to the volume of 70mL, then transferring the reaction solution to a hydrothermal kettle with the volume of 100mL, reacting for 24h at 200 ℃, after the reaction kettle is cooled, washing the product for multiple times by using the deionized water and absolute ethyl alcohol, and putting the washed precipitate into an oven to be dried for 24h at the temperature of 60 ℃. Obtaining the graphene quantum dot-La2O3-ZnFe2O4A composite material. The material is analyzed by a thermogravimetric analysis method, and the content of the graphene quantum dots in the composite material is 1.2 wt%.
The material is made into an indirectly heated element, and the sensitivity of the indirectly heated element to 0.01, 0.1, 1, 10, 100 and 1000ppm acetone gas at the working temperature of 125 ℃ is respectively measured to be 1.5, 3.2, 7.9, 21.3, 62.6 and 136.2. The response time and recovery time for 0.01-1000pp acetone are no longer than 22 seconds and 50 seconds. The sensitivity to 1000ppm ethanol, methanol, acetaldehyde and formaldehyde is respectively 7.7, 6.8, 12.8 and 11.4, and the sensitivity to 1000ppm ammonia, benzene, toluene and hydrogen is not more than 4.
Claims (1)
1. The composite gas-sensitive material with high selectivity to low-concentration acetone is characterized by comprising graphene quantum dots-La2O3-ZnFe2O4A composite material, wherein: the graphene quantum dots account for 0.5-1.5% of the total mass of the material, and the La2O3And ZnFe2O4The molar ratio of (A) to (B) is 2.5 to 4 percent;
the preparation method of the composite gas-sensitive material comprises the following steps:
(1) 0.001mol Zn (NO) is weighed3)2·6H2O、0.002molFe(NO3)3·9H2O、0.00005～0.00008molLa(NO3)3·6H2Dissolving O in 20mL of deionized water; slowly adding 1.5-4.5 ml of graphene quantum dot solution with the concentration of 1mg/g into the solution, stirring for 30min, and carrying out ultrasonic treatment on the mixed solution for 30min to obtain a suspension;
(2) dropwise adding 1mol/L NaOH solution into the suspension obtained in the step (1) until the pH value of the reaction solution is 7.0; adding deionized water to the volume of 70mL, transferring the reaction solution to a hydrothermal kettle with the volume of 100mL, reacting for 24 hours at 180-200 ℃, after the reaction kettle is cooled, washing the product with deionized water and absolute ethyl alcohol, and drying the washed precipitate in a drying oven at 60 ℃ for 24 hours to obtain the graphene quantum dot-La2O3-ZnFe2O4A composite material.
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