CN109490377B - Barium stannate nanotube gas-sensitive material with high gas-sensitive selectivity to acetic acid gas - Google Patents
Barium stannate nanotube gas-sensitive material with high gas-sensitive selectivity to acetic acid gas Download PDFInfo
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Abstract
The invention discloses a barium stannate nanotube gas-sensitive material with high gas-sensitive selectivity to acetic acid gas, and belongs to the technical field of gas-sensitive materials. The material comprises a barium stannate nanotube, the barium stannate nanotube material is prepared by an electrostatic spinning method, the length of the barium stannate nanotube is about 10-100 micrometers, the radius of the barium stannate nanotube is 500-1000 nanometers, and the nanotube wall is composed of barium stannate particles with the average particle size of 50 nanometers. When the working temperature is 245 ℃, the sensitivity of the indirectly heated gas sensor prepared by using the material as a sensitive material to 1000ppm acetic acid reaches 91-96.8, the detection limit to the acetic acid is as low as 0.3ppm, and the response and recovery time to 0.3-1000ppm acetic acid gas respectively do not exceed 50 s. When the element is at the same working temperature of 245 ℃, the sensitivity of the element to 1000ppm of ethanol and acetone is lower than 6.7, namely the barium stannate nanotube gas-sensitive material has high gas-sensitive selectivity to acetic acid gas.
Description
Technical Field
The invention belongs to the technical field of gas-sensitive materials, and particularly relates to a barium stannate nanotube gas-sensitive material with high sensitivity and high selectivity on acetic acid gas.
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
The invention aims to solve the technical problem of providing a high-sensitivity and high-selectivity gas sensitive material for detecting acetic acid gas in air, which can eliminate the interference of acetone, ethanol and the like on the detection of the acetic acid gas and provide a way for rapidly detecting the concentration of the acetic acid gas in the air.
The invention is realized by the following technical scheme.
The invention provides a barium stannate nanotube gas-sensitive material with high gas-sensitive selectivity to acetic acid gas, which comprises a barium stannate nanotube, wherein the length of the barium stannate nanotube is 10-100 microns, the radius of the barium stannate nanotube is 500-1000 nanometers, and the wall of the nanotube is composed of barium stannate particles with the average particle size of 50 nanometers.
The preparation method and the process of the barium stannate nanotube of the invention are as follows: 0.001 mol of Ba (NO)3)2And 0.001 mol SnCl4·5H2Stirring and dissolving O in Dimethylformamide (DMF), adding polyvinylpyrrolidone (PVP, molecular weight of 130000), stirring and dissolving to obtain solution for electrostatic spinning, wherein the mass percentage content of PVP in the solution is 15%, and Ba (NO) in the solution is3)2And SnCl4·5H2The sum of the mass of O accounts for 15 percent of the mass of the solution. Adding the solution into a medical syringe, connecting a needle point and a collection aluminum foil with a high-voltage power supply, wherein the voltage is 17-18kV, the needle point is arranged above, the distance between the needle point and the collection aluminum foil is 13-15 cm, under the action of gravity and an electric field, collecting a precursor of a barium stannate nanotube on the aluminum foil after 4 hours, drying the precursor in air at 200 ℃ for 10 minutes, carrying out heat treatment in a muffle furnace for 2 hours, wherein the heat treatment temperature is 680 and 720 ℃, and the heating rate is 1 ℃/min.
The material of the invention can be used as a sensitive material of an acetic acid 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 slurry electrodes are used at two ends of the alumina tube, gold wires are welded on the electrodes to be used 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 working 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 barium stannate nanotube is prepared by an electrostatic spinning method, the wall of the nanotube is composed of barium stannate nanoparticles, the middle of the nanotube is hollow, gas diffusion is facilitated, and the nanoparticles are beneficial to gas adsorption.
2. The barium stannate nanotube material obtained by the invention has high sensitivity and high selectivity to acetic acid. When the working temperature is 245 ℃, the sensitivity of the indirectly heated gas sensor prepared by the material to 1000ppm acetic acid reaches 91-96.8, the detection limit to the acetic acid is as low as 0.3ppm, the sensitivity to 0.3ppm acetic acid gas reaches 1.2-1.4, and the response and recovery time to 0.3-1000ppm acetic acid gas respectively do not exceed 50 s. When the element is at the same working temperature of 245 ℃, the sensitivity of the element to 1000ppm of ethanol and acetone is lower than 6.7, namely the barium stannate nanotube gas-sensitive material has high gas-sensitive selectivity to acetic acid gas.
Drawings
FIG. 1 is an electron micrograph of barium stannate nanotubes prepared in example 2 of the present invention.
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
0.001 mol of Ba (NO)3)2And 0.001 mol SnCl4·5H2Stirring and dissolving O in Dimethylformamide (DMF), adding polyvinylpyrrolidone (PVP, molecular weight of 130000), stirring and dissolving to obtain solution for electrostatic spinning, wherein the mass percentage content of PVP in the solution is 15%, and Ba (NO) in the solution is3)2And SnCl4·5H2The sum of the mass of O accounts for 15 percent of the mass of the solution. Adding the solution into a medical injector, connecting a needle point and a collecting aluminum foil with a high-voltage power supply, wherein the voltage is 17kV, the needle point is arranged above, the distance between the needle point and the collecting aluminum foil is 13 cm, collecting a precursor of the barium stannate nanotube on the aluminum foil after 4 hours under the action of gravity and an electric field, drying the precursor in air at 200 ℃ for 10 minutes, and carrying out heat treatment in a muffle furnace for 2 hours at the heat treatment temperature of 680 ℃ at the heating rate of 1 ℃/min.
The material is made into an indirectly heated element, and the highest sensitivity of the indirectly heated element to 0.3, 0.5, 1, 10, 100, 500 and 1000ppm of acetic acid gas at the working temperature of 245 ℃ is respectively 1.3, 1.6, 2.2, 10.8, 51.3, 85.0 and 95.3; the sensitivity to 1000ppm acetone and ethanol is respectively 5.0 and 6.1, and the ratio of the sensitivity of the element to 1000ppm acetic acid to the sensitivity to 1000ppm acetone reaches 19.1, which shows that the material has high gas-sensitive selectivity to acetic acid gas; response time and recovery time for 0.3-1000ppm acetic acid do not exceed 46 seconds.
Example 2
0.001 mol of Ba (NO)3)2And 0.001 mol SnCl4·5H2Stirring and dissolving O in Dimethylformamide (DMF), adding polyvinylpyrrolidone (PVP, molecular weight of 130000), stirring and dissolving to obtain solution for electrostatic spinning, wherein the mass percentage content of PVP in the solution is 15%, and Ba (NO) in the solution is3)2And SnCl4·5H2The sum of the mass of O accounts for 15 percent of the mass of the solution. Adding the solution into a medical injector, connecting a needle point and a collecting aluminum foil with a high-voltage power supply, wherein the voltage is 18kV, the needle point is arranged above, the distance between the needle point and the collecting aluminum foil is 15 cm, collecting a precursor of the barium stannate nanotube on the aluminum foil after 4 hours under the action of gravity and an electric field, drying the precursor in air at 200 ℃ for 10 minutes, and carrying out heat treatment in a muffle furnace for 2 hours at the heat treatment temperature of 700 ℃ at the heating rate of 1 ℃/min.
The material is made into an indirectly heated element, and the highest sensitivity of the indirectly heated element to 0.3, 0.5, 1, 10, 100, 500 and 1000ppm of acetic acid gas at the working temperature of 245 ℃ is respectively 1.4, 1.7, 2.5, 12.5, 55, 86.0 and 96.8; the sensitivity to 1000ppm acetone and ethanol is respectively 5.1 and 6.7, and the ratio of the sensitivity of the element to 1000ppm acetic acid to the sensitivity to 1000ppm acetone reaches 19.0, which shows that the material has high gas-sensitive selectivity to acetic acid gas; response time and recovery time for 0.3-1000ppm acetic acid do not exceed 50 seconds.
Example 3
0.001 mol of Ba (NO)3)2And 0.001 mol SnCl4·5H2Stirring and dissolving O in Dimethylformamide (DMF), adding polyvinylpyrrolidone (PVP, molecular weight of 130000), stirring and dissolving to obtain solution for electrostatic spinning, wherein the mass percentage content of PVP in the solution is 15%, and Ba (NO) in the solution is3)2And SnCl4·5H2The sum of the mass of O accounts for 15 percent of the mass of the solution. Adding the solution into a medical syringe, piercing the needle tip and collecting the aluminum foil andthe high-voltage power supply is connected, the voltage is 18kV, the needle point is arranged above, the distance between the needle point and the collection aluminum foil is 15 cm, under the action of gravity and an electric field, a precursor of the barium stannate nanotube is collected on the aluminum foil after 4 hours, the precursor is dried for 10 minutes at 200 ℃ in the air, and is subjected to heat treatment in a muffle furnace for 2 hours, the heat treatment temperature is 720 ℃, and the heating rate is 1 ℃/min.
The material is made into an indirectly heated element, and the highest sensitivity of the indirectly heated element to 0.3, 0.5, 1, 10, 100, 500 and 1000ppm of acetic acid gas at the working temperature of 245 ℃ is measured to be 1.2, 1.5, 2.3, 11.2, 51.1, 81.2 and 91.0 respectively; the sensitivity to 1000ppm acetone and ethanol is respectively 4.5 and 6.2, and the ratio of the sensitivity of the element to 1000ppm acetic acid to the sensitivity to 1000ppm acetone reaches 21.7, which shows that the material has high gas-sensitive selectivity to acetic acid gas; response time and recovery time for 0.3-1000ppm acetic acid do not exceed 45 seconds.
Example 4
0.001 mol of Ba (NO)3)2And 0.001 mol SnCl4·5H2Stirring and dissolving O in Dimethylformamide (DMF), adding polyvinylpyrrolidone (PVP, molecular weight of 130000), stirring and dissolving to obtain solution for electrostatic spinning, wherein the mass percentage content of PVP in the solution is 15%, and Ba (NO) in the solution is3)2And SnCl4·5H2The sum of the mass of O accounts for 15 percent of the mass of the solution. Adding the solution into a medical injector, connecting a needle point and a collecting aluminum foil with a high-voltage power supply, wherein the voltage is 18kV, the needle point is arranged above, the distance between the needle point and the collecting aluminum foil is 15 cm, collecting a precursor of the barium stannate nanotube on the aluminum foil after 4 hours under the action of gravity and an electric field, drying the precursor in air at 200 ℃ for 10 minutes, and carrying out heat treatment in a muffle furnace for 2 hours at the heat treatment temperature of 680 ℃ at the heating rate of 1 ℃/min.
The material is made into an indirectly heated element, and the highest sensitivity of the indirectly heated element to 0.3, 0.5, 1, 10, 100, 500 and 1000ppm of acetic acid gas at the working temperature of 245 ℃ is respectively 1.3, 1.6, 2.6, 10.4, 48.2, 80.1 and 92.3; the sensitivity to 1000ppm acetone and ethanol is respectively 4.3 and 6.4, and the ratio of the sensitivity of the element to 1000ppm acetic acid to the sensitivity to 1000ppm acetone reaches 21.4, which shows that the material has high gas-sensitive selectivity to acetic acid gas; response time and recovery time for 0.3-1000ppm acetic acid do not exceed 50 seconds.
Claims (3)
1. A barium stannate nanotube gas-sensitive material with high gas-sensitive selectivity to acetic acid gas is characterized in that the material comprises a barium stannate nanotube, the length of the barium stannate nanotube is 10-100 micrometers, the radius of the barium stannate nanotube is 500-1000 nanometers, and the nanotube wall is composed of barium stannate particles with the average particle size of 50 nanometers;
the barium stannate nanotube is prepared by an electrostatic spinning method, and the specific preparation steps are as follows:
(1) 0.001 mol of Ba (NO)3)2And 0.001 mol SnCl4·5H2Stirring and dissolving O into dimethylformamide, adding polyvinylpyrrolidone, stirring and dissolving to obtain solution for electrostatic spinning, wherein the mass percentage of polyvinylpyrrolidone in the solution is 15%, and Ba (NO) is added3)2And SnCl4·5H2The sum of the O mass accounts for 15 percent of the solution mass;
(2) adding the solution obtained in the step (1) into a medical injector, connecting a needle point and a collection aluminum foil with a high-voltage power supply, wherein the voltage is 17-18kV, the needle point is arranged above, the distance between the needle point and the collection aluminum foil is 13-15 cm, and collecting a precursor of a barium stannate nanotube on the aluminum foil after 4 hours under the action of gravity and an electric field;
(3) and (3) drying the precursor obtained in the step (2) in air at 200 ℃ for 10 minutes, and carrying out heat treatment in a muffle furnace for 2 hours at the heat treatment temperature of 680-720 ℃ and the heating rate of 1 ℃/min.
2. The barium stannate nanotube gas sensitive material of claim 1, wherein the polyvinylpyrrolidone of step (1) has a molecular weight of 130000.
3. The barium stannate nanotube gas sensitive material of claim 1, which is used as a gas sensor made of an acetic acid gas sensitive element.
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