CN111239205A - Based on CdSnO3Isopropyl alcohol gas sensor of sensitive layer and preparation method thereof - Google Patents
Based on CdSnO3Isopropyl alcohol gas sensor of sensitive layer and preparation method thereof Download PDFInfo
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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
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
Abstract
CdS quantum dot modification-based porous cubic structure CdSnO3An isopropanol gas sensor with nano particles as a sensitive layer and a preparation method thereof belong to the technical field of gas sensors. The sensor is sequentially composed of Al with Pd metal interdigital electrodes from bottom to top2O3Substrate, metal interdigital electrode on Pd and Al2O3CdS quantum dot modified porous cubic structure CdSnO prepared by coating technology on substrate3A nanoparticle sensitive layer; the invention adopts CdS quantum dot modified porous cubic structure CdSnO3The nano-particles are used as sensitive materials, and not only are amorphous CdSnO applied3The advantage of the surface dangling bond of the nano-particles can also effectively utilize the larger specific surface area of the quantum dot to improve the gas-sensitive response. Meanwhile, the method has simple process, and the prepared device has small volume and is suitable for mass production, thereby having important application value.
Description
Technical Field
The invention belongs to the technical field of gas sensors, and particularly relates to CdS quantum dot modification-based porous cubic structure CdSnO3An isopropanol gas sensor with nano particles as a sensitive layer and a preparation method thereof.
Background
With the rapid development of informatization and digitization, people enjoy the great abundance of material wealth and are suffering from the harm brought to people by environmental pollution. More and more toxic and harmful gases are discharged into the air, such as sulfur dioxide and nitrogen oxides in coal combustion and automobile exhaust, organic volatile toxic gases such as benzene, formaldehyde and xylene released from building materials, and flammable and explosive gases such as ethanol, hydrogen and isopropanol discharged from chemical production. Once leaked, the flammable, explosive, toxic and harmful gases not only cause serious pollution to the environment, but also seriously threaten the health of human beings. Therefore, in consideration of environmental protection and personal safety, it is very important to research and develop some high-performance gas sensors with high responsiveness, good selectivity and fast detection speed.
Isopropyl alcohol is a colorless, flammable, toxic and pungent organic volatile compound that is commonly used as an industrial solvent, cleaning agent and extractant. When the isopropanol gas leaks into the air and reaches a certain concentration, the isopropanol gas can explode when meeting open fire, thereby threatening the life health and property safety of human beings. If the isopropanol leakage can be detected and an alarm is given out at the initial stage (the concentration is lower than the lower explosion limit) of the isopropanol leakage, the gas leakage can be quickly controlled, the explosion is avoided, and the life health and property safety of people are protected. Therefore, the isopropanol gas sensor with high responsiveness, low detection lower limit and high response speed is researched and developed, and has important practical significance.
The gas sensor directly adsorbs detection gas by using a sensitive material, so that the electrical property and the like of the material are changed, and the gas concentration is detected by detecting the change of an output signal of a sensitive element of a peripheral circuit. There are many materials used for gas sensing, and at present, metal oxide semiconductor sensitive materials are mainly used. The morphology of the material is closely related to the gas-sensitive performance of the semiconductor sensitive material, and the surface modifier can improve the gas-sensitive performance by improving the surface activity and the catalytic activity of the material. Therefore, the gas sensing performance is often improved by synthesizing sensitive materials with different morphologies and selecting different modifying materials. In addition to this, the structure of the sensitive material also has an effect on the gas-sensing properties. Among them, the heterostructure is widely studied and applied.
Disclosure of Invention
The invention aims to provide CdS quantum dot modified porous cubic structure CdSnO3An isopropanol gas sensor with nano particles as a sensitive layer and a preparation method thereof. The method is simple and easy to implement, few in working procedures, low in cost and low in equipment requirement, can improve the gas-sensitive response of the sensor to the isopropanol gas, is suitable for mass production, and has important application value.
The invention relates to CdS quantum dot modification-based porous cubic structure CdSnO3The isopropanol gas sensor with nano particles as a sensitive layer is composed of Al with Pd metal interdigital electrodes from bottom to top in sequence2O3Substrate, metal interdigital electrode on Pd and Al2O3CdS quantum dot modified porous cubic structure CdSnO prepared by coating technology on substrate3A nanoparticle sensitive layer; CdS quantum dot modified porous cubic structure CdSnO3The particle size of the nano particles is 80-100 nm, the width and the spacing of the Pd metal interdigital electrodes are 0.15-0.20 mm, and the thickness is 100-150 nm.
The CdS quantum dot modification-based porous cubic structure CdSnO3The preparation method of the isopropanol gas sensor with the nano particles as the sensitive layer comprises the following steps:
(1) treatment of Pd metal interdigital electrode
Firstly, respectively wiping Al with Pd metal interdigital electrode by using ethanol and acetone cotton balls2O3Cleaning the substrate, and then putting Al with Pd metal interdigital electrode2O3Sequentially placing the substrate in acetone, ethanol and deionized water, respectively ultrasonically cleaning for 5-10 minutes, and finally cleaning inDrying at 100-120 ℃;
applying screen printing technology to Al2O3Preparing a Pd metal interdigital electrode on a substrate: mixing the ink [ Jiahua JX07500487]: pd powder: the diluent is mixed according to the mass ratio of 1: 1: 2, stirring and preparing into paste, then injecting the paste onto a silk screen plate with interdigital electrode patterns, scraping the paste under the conditions of an inclination angle of 30-45 degrees and a pressure of 5-10 newtons, and carrying out Al deposition2O3Printing electrodes on the substrate, drying, and finishing the preparation of the Pd metal interdigital electrode after ultraviolet curing; the width and the electrode spacing of the Pd metal interdigital electrode are both 0.15-0.20 mm, and the thickness is 100-150 nm;
(2) CdS quantum dot modified porous cubic structure CdSnO3Preparation of nanoparticles
① porous cubic structure CdSnO3Preparing nano particles:
weighing 10-30 mL of deionized water at room temperature, adding 0.2-0.4 g of cadmium nitrate and 0.1-0.3 g of citric acid monohydrate, and stirring for 10-20 minutes to form a solution A; then dissolving 0.3-0.5 g of tin tetrachloride pentahydrate in 5-15 mL of absolute ethanol to form a solution B; mixing the solution A and the solution B, adding 0.5-0.6 g of sodium hydroxide, adding 20-40 mL of deionized water into the obtained mixed solution, and stirring at room temperature for 1-3 hours; transferring the obtained mixed solution into a reaction kettle, reacting at 170-200 ℃ for 12-24 hours, cooling to room temperature, centrifugally cleaning the product by deionized water and absolute ethyl alcohol, and drying the centrifugal product at 60-80 ℃ for 24-30 hours; finally calcining for 5-8 hours at 500-650 ℃ to obtain the porous cubic structure CdSnO3A nanoparticle;
② CdS quantum dot modified porous cubic structure CdSnO3Preparing nano particles:
at room temperature, the porous cubic structure CdSnO prepared in the step ①3Adding the nano particles into 10-20 mL of deionized water, and stirring for 2-4 hours to enable the porous cubic structure CdSnO3The nanoparticles are uniformly dispersed in the solution; then 0.01-0.06 g of cadmium nitrate is added into the mixed solutionMixing with 0.002-0.01 g thioacetamide and stirring for 1-2 hr to homogenize the solution; then heating the solution in water bath at 40-60 ℃, and stirring for 10-20 minutes; finally, centrifugally cleaning the obtained product by using deionized water, and drying the centrifugal product at room temperature to obtain CdS quantum dot modified porous cubic structure CdSnO3A nanoparticle;
(3) CdS quantum dot modification-based porous cubic structure CdSnO3Preparation of isopropanol gas sensor with nano-particles as sensitive layer
The prepared CdS quantum dot modified porous cubic structure CdSnO3Putting the nano particles into a mortar, and grinding for 10-20 minutes to obtain uniformly dispersed nano powder; then, dripping deionized water into the mortar, and continuously grinding for 10-20 minutes to obtain viscous slurry; dipping a small amount of slurry by a medicine spoon, and coating the slurry on Al with Pd metal interdigital electrodes2O3Drying the substrate at 60-80 ℃ to obtain CdSnO with a porous cubic structure modified by CdS quantum dots with the coating thickness of 2-4 mu m3A nanoparticle sensitive layer; finally, in an environment with the relative humidity of 30-55% RH and the temperature of 20-35 ℃, aging is carried out for 48-72 hours under the direct current of 70-100 mA, and thus the porous cubic structure CdSnO modified based on CdS quantum dots is obtained3The nanometer particle is an isopropanol gas sensor of a sensitive layer.
After the gas sensor was prepared, the isopropyl alcohol gas-sensitive performance was tested (CGS-1 TP type gas-sensitive performance tester, ehrit technologies ltd, beijing).
The invention has the advantages and positive effects that: the invention adopts CdS quantum dot modified porous cubic structure CdSnO3The nano-particles are used as sensitive materials, and not only are amorphous CdSnO applied3The advantages of the surface dangling bond of the nano-particles can also effectively utilize the larger specific surface area of the quantum dots to improve the gas-sensitive response, and the method has good detection performance on the isopropanol gas, and simultaneously has simple process, small volume of the prepared device and suitability for mass production, thereby having important application value.
Drawings
FIG. 1 shows CdS quantum dot modified porous cubic structure CdSnO3SEM topography of nanoparticles, corresponding to example 1;
FIG. 2 is an enlarged view of a part of FIG. 1, corresponding to embodiment 1;
FIG. 3 shows CdS quantum dot modified porous cubic structure CdSnO3TEM topography of nanoparticles, corresponding to example 1;
FIG. 4 shows CdS quantum dot modified porous cubic structure CdSnO3XRD pattern of nanoparticles, corresponding to example 1;
FIG. 5 is a schematic structural view of an isopropyl alcohol gas sensor according to the present invention, which corresponds to example 1;
FIG. 6 is a graph showing the relationship between the responsivity of the prepared isopropanol gas sensor at a working temperature of 138 ℃ and the concentration of isopropanol, wherein the responsivity is represented by the ratio of the resistance value of the device in the air to the resistance value of the device in the gas to be measured, which corresponds to example 1;
FIG. 7 is a graph showing the response recovery of an IPA gas sensor prepared according to the present invention at an operating temperature of 138 deg.C and an IPA concentration of 5ppm, which corresponds to example 1;
FIG. 8 is a graph showing the response recovery of an IPA gas sensor prepared according to the present invention at an operating temperature of 138 deg.C and an IPA concentration of 20ppm, which corresponds to example 2;
FIG. 9 is a graph showing the response recovery of an IPA gas sensor prepared according to the present invention at an operating temperature of 138 deg.C and an IPA concentration of 100ppm, which corresponds to example 3;
FIG. 10 is a schematic diagram showing the selective characteristics of the prepared isopropanol gas sensor of the present invention at a working temperature of 138 ℃ and a gas concentration of 100ppm, corresponding to example 1.
From FIGS. 1 and 2, CdS quantum dot modified CdSnO3The nano particles are in a regular cubic structure, and the particle size is about 80-100 nm.
From FIG. 3, it can be seen that CdS quantum dot modified porous cubic structure CdSnO3The interior of the nano-particles is of a porous structure.
From FIG. 4 can be seenIt is seen that the XRD spectrum shows the presence of CdSnO3And the characteristic peak of CdS, indicating that the sample contains CdSnO3And CdS.
As shown in FIG. 5, the gas sensor is made of Al2O3Substrate 1, Pd metal interdigital electrode 3 and CdS quantum dot modified CdSnO3A nanoparticle sensitive layer 2.
As shown in FIG. 6, when the gas sensor is operated at 138 ℃, the sensitivity of the gas sensor increases with the increase of the concentration of the isopropanol, and the curve shows a good linear relationship in the concentration range of 1-50 ppm.
As shown in fig. 7, when the gas sensor was operated at 138 deg.c and the concentration of isopropyl alcohol was 5ppm, the response of the gas sensor was about 8s and the recovery time of the gas sensor was about 9 s. Corresponding to example 1.
As shown in fig. 8, when the gas sensor was operated at 138 deg.c and the concentration of isopropyl alcohol was 20ppm, the response of the gas sensor was about 9s and the recovery time of the gas sensor was about 11 s. Corresponding to example 2.
As shown in fig. 9, when the gas sensor was operated at 138 deg.c and the concentration of isopropyl alcohol was 100ppm, the response of the gas sensor was about 11s and the recovery time of the gas sensor was about 10 s. Corresponding to example 3.
As shown in fig. 10, when the gas sensor was operated at 138 ℃ and the gas concentration was 100ppm, the response value of the gas sensor to isopropyl alcohol was higher than that of the other detection gases. The gas sensor showed good selectivity.
Detailed Description
Example 1:
firstly, respectively wiping Al with a Pd metal interdigital electrode which is prepared by a silk-screen printing technology and has the width of 3mm and the length of 4mm by using acetone and ethanol cotton balls2O3Cleaning the substrate, and then putting Al with Pd metal interdigital electrode2O3The substrate is sequentially placed in acetone, ethanol and deionized water, respectively ultrasonically cleaned for 5 minutes, and finally dried at 100 ℃ for later use.
Wherein, the screen printing technology is adopted to print Al2O3SubstratePreparing Pd metal interdigital electrode according to ink [ Jiahua JX07500487]: pd powder: the mass ratio of the diluent is 1: 1: 2, stirring to prepare paste; then, the paste was poured onto a screen plate having an interdigital electrode pattern, scraped at an inclination angle of 30 ℃ and under a pressure of 5N, and applied to Al2O3And the substrate is provided with a printed electrode and is dried, and the Pd metal interdigital electrode is prepared after ultraviolet light curing. The width and the electrode spacing of the Pd metal interdigital electrode are both 0.15mm, and the thickness is 100 nm.
Method for preparing porous cubic structure CdSnO by solvothermal method3Nano-particles: weighing 10mL of deionized water at room temperature, adding 0.2g of cadmium nitrate and 0.1g of citric acid monohydrate, and stirring for 20 minutes to form a solution A; 0.3g of tin tetrachloride pentahydrate was then dissolved in 5mL of absolute ethanol to form solution B; mixing the solution A and the solution B, adding 0.5g of sodium hydroxide, adding 20mL of deionized water into the mixed solution, and stirring at room temperature for 1 hour; transferring the obtained mixed solution into a reaction kettle to react for 24 hours at the temperature of 170 ℃, cooling to room temperature, centrifugally cleaning the product by deionized water and absolute ethyl alcohol, and drying the centrifugal product for 24 hours at the temperature of 80 ℃; finally calcining the mixture for 5 hours at 500 ℃ to obtain the porous cubic structure CdSnO3And (3) nanoparticles.
CdS quantum dot modification process: 0.05g of porous cubic CdSnO is added under room temperature3Adding the nano particles into 20mL of deionized water, and stirring for 2 hours to ensure that the porous cubic structure of CdSnO3The nanoparticles are uniformly dispersed in the solution; then adding 0.01g of cadmium nitrate and 0.002g of thioacetamide into the mixed solution, and continuing stirring for 1 hour to ensure that the solution is uniform; then heating the solution in water bath at 40 ℃, and stirring for 10 minutes; and finally, centrifugally cleaning the obtained product by using deionized water, and drying the centrifugal product at room temperature to obtain 0.05g of CdS quantum dot modified porous cubic structure CdSnO3And (3) nanoparticles.
CdS quantum dot modification-based porous cubic structure CdSnO3Preparing an isopropanol gas sensor with nanoparticles as a sensitive layer:
the dried CdS quantum dots are modified to form a porous cubic structure CdSnO3Putting the nano particles into a mortar, and grinding for 10 minutes to obtain uniformly dispersed nano powder; then, deionized water (CdS quantum dot modified porous cubic structure CdSnO) is dripped into the mortar3The mass ratio of the nanoparticles to the water is 5: 2) then, continuously grinding for 10 minutes to obtain viscous slurry; dipping a small amount of slurry by a medicine spoon, and coating the slurry on Al with Pd metal interdigital electrodes2O3Drying the substrate at 60 ℃ to obtain the CdSnO with the porous cubic structure modified by CdS quantum dots with the coating thickness of 2 mu m3A nanoparticle sensitive layer; finally, aging the CdS quantum dot modified porous cubic structure CdSnO for 48 hours under the direct current of 100mA in the environment with the relative humidity of 40% RH and the temperature of 25 ℃ to obtain the CdS quantum dot modified porous cubic structure CdSnO3The gas sensor takes nano particles as a sensitive layer and metal Pd as an interdigital electrode.
The porous cubic structure CdSnO modified by CdS quantum dots prepared in the above embodiments3The gas-sensitive performance of the gas sensor taking the nano-particles as the sensitive layer and the metal Pd as the interdigital electrode is tested by a CGS-1TP type gas-sensitive performance tester of Elite technologies, Inc. of Beijing. The gas-sensitive performance indexes are as follows:
sensitivity was 1.91(5ppm isopropanol);
the response time was 8 seconds and the recovery time was 9 seconds.
Example 2:
firstly, respectively wiping Al with a Pd metal interdigital electrode which is prepared by a silk-screen printing technology and has the width of 3mm and the length of 4mm by using acetone and ethanol cotton balls2O3Cleaning the substrate, and then putting Al with Pd metal interdigital electrode2O3The substrate is sequentially placed in acetone, ethanol and deionized water, respectively ultrasonically cleaned for 5 minutes, and finally dried at 100 ℃ for later use.
Wherein, the screen printing technology is adopted to print Al2O3Preparing Pd metal interdigital electrode on the substrate according to the ink [ Jiahua JX07500487]: pd powder: the mass ratio of the diluent is 1: 1: 2, stirring to prepare paste; then the slurry is mixedInjecting the paste onto a screen plate with interdigital electrode pattern, scraping the paste under the conditions of 45-degree inclination angle and 5-Newton pressure, and applying Al2O3The substrate is provided with printed electrodes and is dried, and the width and the electrode spacing of the Pd metal interdigital electrodes prepared by the Pd metal interdigital electrodes after ultraviolet light curing are both 0.15mm, and the thickness is 100 nm.
Method for preparing porous cubic structure CdSnO by solvothermal method3Nano-particles: weighing 10mL of deionized water at room temperature, adding 0.2g of cadmium nitrate and 0.3g of citric acid monohydrate, and stirring for 10 minutes to form a solution A; 0.5g of tin tetrachloride pentahydrate was then dissolved in 10mL of absolute ethanol to form solution B; mixing the solution A and the solution B, adding 0.5g of sodium hydroxide, adding 20mL of deionized water into the mixed solution, and stirring at room temperature for 2 hours; transferring the obtained mixed solution into a reaction kettle, reacting for 24 hours at 170 ℃, cooling to room temperature, centrifugally cleaning the product by deionized water and absolute ethyl alcohol, and drying the centrifugal product for 30 hours at 80 ℃; finally calcining for 8 hours at 500 ℃ to obtain the porous cubic structure CdSnO3And (3) nanoparticles.
CdS quantum dot modification process: 0.05g of porous cubic CdSnO is added under room temperature3Adding the nano particles into 10mL of deionized water, and stirring for 2 hours to ensure that the porous cubic structure of CdSnO3The nanoparticles are uniformly dispersed in the solution; then adding 0.03g of cadmium nitrate and 0.005g of thioacetamide into the mixed solution, and continuing stirring for 1 hour to ensure that the solution is uniform; then heating the solution in water bath at 40 ℃, and stirring for 20 minutes; and finally, centrifugally cleaning the obtained product by using deionized water, and drying the centrifugal product at room temperature to obtain 0.05g of CdS quantum dot modified porous cubic structure CdSnO3And (3) nanoparticles.
CdS quantum dot modification-based porous cubic structure CdSnO3Preparing an isopropanol gas sensor with nanoparticles as a sensitive layer:
the dried CdS quantum dots are modified to form a porous cubic structure CdSnO3The nano particles are put into a mortar and ground for 10 minutes to obtain the mixtureUniformly dispersed nano-powder; then, deionized water (CdS quantum dot modified porous cubic structure CdSnO) is dripped into the mortar3The mass ratio of the nanoparticles to the water is 5: 2) then, continuously grinding for 20 minutes to obtain viscous slurry; dipping a small amount of slurry by a medicine spoon, and coating the slurry on Al with Pd metal interdigital electrodes2O3Drying the substrate at 70 ℃ to obtain the CdSnO with the porous cubic structure modified by CdS quantum dots with the coating thickness of 3 mu m3A nanoparticle sensitive layer; finally, aging the CdS quantum dot modified porous cubic structure CdSnO for 48 hours under the direct current of 80mA in the environment with the relative humidity of 45 percent RH and the temperature of 28 ℃ to obtain the CdSnO quantum dot modified porous cubic structure CdSnO3The gas sensor takes nano particles as a sensitive layer and metal Pd as an interdigital electrode.
The porous cubic structure CdSnO modified by CdS quantum dots prepared in the above embodiments3The gas-sensitive performance of the gas sensor taking the nano-particles as the sensitive layer and the metal Pd as the interdigital electrode is tested by a CGS-1TP type gas-sensitive performance tester of Elite technologies, Inc. of Beijing. The gas-sensitive performance indexes are as follows:
sensitivity was 5.53(20ppm isopropanol);
the response time was 9 seconds and the recovery time was 11 seconds.
Example 3:
firstly, respectively wiping Al with a Pd metal interdigital electrode which is prepared by a silk-screen printing technology and has the width of 3mm and the length of 4mm by using acetone and ethanol cotton balls2O3Cleaning the substrate, and then putting Al with Pd metal interdigital electrode2O3The substrate is sequentially placed in acetone, ethanol and deionized water, respectively ultrasonically cleaned for 5 minutes, and finally dried at 100 ℃ for later use.
Wherein, the screen printing technology is adopted to print Al2O3Preparing Pd metal interdigital electrode on the substrate according to the ink [ Jiahua JX07500487]: pd powder: the mass ratio of the diluent is 1: 1: 2, stirring to prepare paste; then, the paste was poured onto a screen plate having an interdigital electrode pattern, scraped at an inclination angle of 30 ℃ and under a pressure of 10N, and applied to Al2O3The substrate isAnd printing electrodes and drying, and after ultraviolet curing, finishing the preparation of the Pd metal interdigital electrode, wherein the width and the electrode spacing of the Pd metal interdigital electrode are both 0.15mm, and the thickness is 100 nm.
Method for preparing porous cubic structure CdSnO by solvothermal method3Nano-particles: weighing 30mL of deionized water at room temperature, adding 0.4g of cadmium nitrate and 0.3g of citric acid monohydrate, and stirring for 20 minutes to form a solution A; 0.5g of tin tetrachloride pentahydrate was then dissolved in 15mL of absolute ethanol to form solution B; mixing the solution A and the solution B, adding 0.6g of sodium hydroxide, adding 40mL of deionized water into the mixed solution, and stirring at room temperature for 3 hours; transferring the obtained mixed solution into a reaction kettle, reacting for 12 hours at 170 ℃, cooling to room temperature, centrifugally cleaning the product by deionized water and absolute ethyl alcohol, and drying the centrifugal product for 24 hours at 60 ℃; finally calcining at 650 ℃ for 5 hours to obtain the porous cubic structure CdSnO3And (3) nanoparticles.
CdS quantum dot modification process: 0.05g of porous cubic CdSnO is added under room temperature3Adding the nano particles into 10mL of deionized water, and stirring for 3 hours to ensure that the porous cubic structure of CdSnO3The nanoparticles are uniformly dispersed in the solution; then adding 0.06g of cadmium nitrate and 0.01g of thioacetamide into the mixed solution, and continuing stirring for 2 hours to ensure that the solution is uniform; then heating the solution in water bath at 60 ℃, and stirring for 10 minutes; and finally, centrifugally cleaning the obtained product by using deionized water, and drying the centrifugal product at room temperature to obtain 0.05g of CdS quantum dot modified porous cubic structure CdSnO3And (3) nanoparticles.
CdS quantum dot modification-based porous cubic structure CdSnO3Preparing an isopropanol gas sensor with nanoparticles as a sensitive layer:
the dried CdS quantum dots are modified to form a porous cubic structure CdSnO3Putting the nano particles into a mortar, and grinding for 20 minutes to obtain uniformly dispersed nano powder; then, deionized water (CdS quantum dot modified porous cubic structure CdSnO) is dripped into the mortar3The mass ratio of the nano particles to the water is5: 2) then, continuously grinding for 10 minutes to obtain viscous slurry; dipping a small amount of slurry by a medicine spoon, and coating the slurry on Al with Pd metal interdigital electrodes2O3Drying the substrate at 80 ℃ to obtain CdSnO with a porous cubic structure modified by CdS quantum dots with the coating thickness of 4 mu m3A nanoparticle sensitive layer; finally, aging for 72 hours under 70mA direct current in an environment with the relative humidity of 55% RH and the temperature of 30 ℃ so as to obtain the CdSnO modified by CdS quantum dots and having a porous cubic structure3The gas sensor takes nano particles as a sensitive layer and metal Pd as an interdigital electrode.
The porous cubic structure CdSnO modified by CdS quantum dots prepared in the above embodiments3The gas-sensitive performance of the gas sensor taking the nano-particles as the sensitive layer and the metal Pd as the interdigital electrode is tested by a CGS-1TP type gas-sensitive performance tester of Elite technologies, Inc. of Beijing. The gas-sensitive performance indexes are as follows:
sensitivity was 20.12(100ppm isopropanol);
the response time was 11 seconds and the recovery time was 10 seconds.
The above description is only an embodiment of the present invention, and the scope of the present invention should not be limited thereto, but all equivalent changes and modifications made within the scope of the present invention should still fall within the scope covered by the present invention.
Claims (4)
1. CdS quantum dot modification-based porous cubic structure CdSnO3The isopropanol gas sensor with the nano particles as the sensitive layer is characterized in that: from bottom to top in turn by Al with Pd metal interdigital electrodes2O3Substrate, metal interdigital electrode on Pd and Al2O3CdS quantum dot modified porous cubic structure CdSnO prepared on substrate3A nanoparticle sensitive layer; CdS quantum dot modified porous cubic structure CdSnO3The nanoparticles are prepared by the following steps,
① porous cubic structure CdSnO3Preparing nano particles:
weighing at room temperature10-30 mL of deionized water, then adding 0.2-0.4 g of cadmium nitrate and 0.1-0.3 g of citric acid monohydrate, and stirring for 10-20 minutes to form a solution A; then dissolving 0.3-0.5 g of tin tetrachloride pentahydrate in 5-15 mL of absolute ethanol to form a solution B; mixing the solution A and the solution B, adding 0.5-0.6 g of sodium hydroxide, adding 20-40 mL of deionized water into the obtained mixed solution, and stirring at room temperature for 1-3 hours; transferring the obtained mixed solution into a reaction kettle, reacting at 170-200 ℃ for 12-24 hours, cooling to room temperature, centrifugally cleaning the product by deionized water and absolute ethyl alcohol, and drying the centrifugal product at 60-80 ℃ for 24-30 hours; finally calcining for 5-8 hours at 500-650 ℃ to obtain the porous cubic structure CdSnO3A nanoparticle;
② CdS quantum dot modified porous cubic structure CdSnO3Preparing nano particles:
at room temperature, the porous cubic structure CdSnO prepared in the step ①3Adding the nano particles into 10-20 mL of deionized water, and stirring for 2-4 hours to enable the porous cubic structure CdSnO3The nanoparticles are uniformly dispersed in the solution; then adding 0.01-0.06 g of cadmium nitrate and 0.002-0.01 g of thioacetamide into the mixed solution, and continuously stirring for 1-2 hours to ensure that the solution is uniform; then heating the solution in water bath at 40-60 ℃, and stirring for 10-20 minutes; finally, centrifugally cleaning the obtained product by using deionized water, and drying the centrifugal product at room temperature to obtain CdS quantum dot modified porous cubic structure CdSnO3And (3) nanoparticles.
2. The CdS quantum dot modified porous cubic structure CdSnO as claimed in claim 13The isopropanol gas sensor with the nano particles as the sensitive layer is characterized in that: CdS quantum dot modified porous cubic structure CdSnO3The particle size of the nano particles is 80-100 nm, the width and the spacing of the Pd metal interdigital electrodes are 0.15-0.20 mm, the thickness is 100-150 nm, and the thickness of the sensitive layer is 2-4 mu m.
3. The method of claim 1The CdS quantum dot modified porous cubic structure CdSnO3The preparation method of the isopropanol gas sensor with the nano particles as the sensitive layer comprises the following steps:
(1) treatment of Pd metal interdigital electrode
Firstly, respectively wiping Al with Pd metal interdigital electrode by using ethanol and acetone cotton balls2O3Cleaning the substrate, and then putting Al with Pd metal interdigital electrode2O3Sequentially placing the substrate in acetone, ethanol and deionized water, respectively ultrasonically cleaning for 5-10 minutes, and finally drying at 100-120 ℃;
(2) CdS quantum dot modification-based porous cubic structure CdSnO3Preparation of isopropanol gas sensor with nano-particles as sensitive layer
The prepared CdS quantum dot modified porous cubic structure CdSnO3Putting the nano particles into a mortar, and grinding for 10-20 minutes to obtain uniformly dispersed nano powder; then, dripping deionized water into the mortar, and continuously grinding for 10-20 minutes to obtain viscous slurry; dipping a small amount of slurry by a medicine spoon, and coating the slurry on Al with Pd metal interdigital electrodes2O3Drying the substrate at 60-80 ℃ to obtain CdSnO with a porous cubic structure modified by CdS quantum dots with the coating thickness of 2-4 mu m3A nanoparticle sensitive layer; finally, in an environment with the relative humidity of 30-55% RH and the temperature of 20-35 ℃, aging is carried out for 48-72 hours under the direct current of 70-100 mA, and thus the porous cubic structure CdSnO modified based on CdS quantum dots is obtained3The nanometer particle is an isopropanol gas sensor of a sensitive layer.
4. The CdS quantum dot modified porous cubic structure CdSnO as claimed in claim 33The preparation method of the isopropanol gas sensor with the nano particles as the sensitive layer is characterized by comprising the following steps: CdS quantum dot modified porous cubic structure CdSnO in step (2)3The mass ratio of the nano particles to the deionized water is 5: 1 to 3.
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