CN109752415B - Ethyl acetate gas sensor and preparation method thereof - Google Patents
Ethyl acetate gas sensor and preparation method thereof Download PDFInfo
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Abstract
PrFeO as one new kind of catalyst3Modified core-shell octahedral structure Fe2O3An ethyl acetate gas sensor with nano particles as a sensitive layer and a preparation method thereof belong to the technical field of gas sensors. From Al with Pd metal interdigital electrodes2O3Substrate of Pd goldInterdigital electrode and Al2O3PrFeO prepared on a substrate by adopting coating technology3Modified core-shell octahedral structure Fe2O3A nanoparticle sensitive layer; the particle size of the nano-particles is 500 nm-700 nm, and a large amount of PrFeO3The nano particles grow on the core-shell octahedral structure Fe2O3On the surface of (a); the method is simple and easy to implement, few in working procedures, low in cost and low in equipment requirement, and the prepared ethyl acetate gas sensor is quick in gas-sensitive response, suitable for mass production and has important application value.
Description
Technical Field
The invention belongs to the technical field of gas sensors, and particularly relates to a sensor using PrFeO3Modified core-shell octahedral structure Fe2O3An ethyl acetate gas sensor with nano particles as a sensitive layer and a preparation method thereof.
Background
With the rapid development of industrialization and modernization processes, production safety and environmental problems are increasingly highlighted while material wealth is greatly enriched. More and more toxic and harmful gases are discharged into the air, such as carbon monoxide, sulfur dioxide, nitrogen oxides and the like in coal combustion and automobile exhaust, and benzene, formaldehyde, xylene and the like which are organic volatile toxic gases released from building materials. Once generated or leaked, the flammable, explosive, toxic and harmful gases not only cause serious pollution to the environment, but also threaten the health and life of people. Therefore, in consideration of environmental protection and personal safety, it is necessary to research and develop some gas sensors with high responsiveness and high detection speed.
Ethyl acetate is commonly used as an industrial solvent, a binder and a perfume raw material, is colorless and sweet, flammable and explosive toxic gas, and is easy to form explosive mixtures with air. When ethyl acetate leaks into the air and reaches a certain concentration, the ethyl acetate can explode when meeting open fire, thereby threatening the safety of life and property of people. If the ethyl acetate can be detected and an alarm is given out when the concentration is lower than the upper explosion limit in the initial stage of leakage, the explosion can be effectively avoided, and the life and property safety of people can be protected. Therefore, the development of the ethyl acetate gas sensor with high responsiveness, low detection lower limit and high response speed is of great 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 through a peripheral circuit.
There are many materials used for gas sensing, and at present, oxide semiconductor sensitive materials are mainly used. Oxide semiconductor sensitive materials with different morphologies have great influence on the gas-sensitive performance, so that the gas-sensitive performance is often improved by synthesizing the sensitive materials with different morphologies. 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 a new compound of PrFeO3Modified core-shell octahedral structure Fe2O3An ethyl acetate 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, and the prepared ethyl acetate gas sensor is quick in gas-sensitive response, suitable for mass production and has important application value.
The invention relates to a new compound of PrFeO3Modified core-shell octahedral structure Fe2O3The ethyl acetate gas sensor with nano particles as a sensitive layer sequentially comprises Al with Pd metal interdigital electrodes from bottom to top2O3Substrate, metal interdigital electrode on Pd and Al2O3The sensitive layer prepared by coating technology on the substrate; the method is characterized in that: with PrFeO3Modified core-shell octahedral structure Fe2O3The nano particles are a sensitive layer, the particle size of the nano particles is 500 nm-700 nm, and a large amount of PrFeO3The nano particles grow on the core-shell octahedral structure Fe2O3On the surface of (a); the width and the spacing of the Pd metal interdigital electrodes are 0.15-0.20 mm, and the thickness is 100-150 nm; and PrFeO3Modified core-shell octahedral structure Fe2O3The nano-particle sensitive layer is prepared by the following steps,
preparing an organic metal framework nano material MIL-53 with an octahedral structure: weighing 30-50 mL of dimethylformamide at room temperature, adding 0.2-0.4 g of terephthalic acid and 0.6-0.8 g of ferric chloride hexahydrate, and stirring for 10-30 minutes; transferring the obtained mixed solution into a reaction kettle, reacting at 120-150 ℃ for 20-24 hours, cooling the obtained product to room temperature, centrifugally cleaning the product with deionized water, and drying at 70-80 ℃ for 20-30 hours to obtain an octahedral organic metal framework nano material MIL-53;
②PrFeO3modified core-shell octahedral structure Fe2O3Preparing a nano material: adding the octahedral organic metal framework nano material MIL-53 nano material prepared in the step I into 15-25 mL of absolute ethyl alcohol at room temperature, and stirring for 1-2 hours to uniformly disperse the octahedral organic metal framework nano material MIL-53 in the solution; then adding 0.04-0.16 g of praseodymium nitrate hexahydrate and 0.5-0.7 g of sodium citrate into the mixed solution, and continuing stirring for 2-3 hours to make the solution uniform; and finally, centrifugally cleaning the obtained product by using deionized water, drying the centrifugal product at room temperature, then placing the obtained product in a high-temperature tube furnace, vacuumizing, filling mixed gas (the volume flow ratio of nitrogen to oxygen is 9: 1-1.2), and calcining at 350-400 DEG CSintering for 2-3 hours to obtain PrFeO3Modified core-shell octahedral structure Fe2O3Nanoparticle sensitive layer material.
The invention adopts PrFeO3Modified core-shell octahedral structure Fe2O3The ethyl acetate gas sensor with the nano particles as the sensitive layer comprises the following preparation steps:
1) pd metal interdigital electrode treatment
Firstly, respectively wiping Al with Pd metal interdigital electrode prepared by screen printing technology by using acetone and ethanol cotton balls2O3Cleaning the substrate, and adding Al2O3Sequentially placing the substrate in acetone, ethanol and deionized water, respectively ultrasonically cleaning for 5-10 minutes, and finally drying at 100-120 ℃;
preparing a Pd metal interdigital electrode by adopting a screen printing technology, and preparing the Pd metal interdigital electrode according to an ink [ Jiahua JX07500487 ]: pd powder: the mass ratio of the diluent is 1: 1: 2, stirring the printing ink to prepare paste; then, injecting the paste onto a wire mesh 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, printing electrodes, drying, and curing by ultraviolet light to finish the preparation of the Pd metal interdigital electrode, wherein the finger width and the electrode spacing of the Pd metal interdigital electrode are 0.15-0.20 mm, and the thickness of the Pd metal interdigital electrode is 100-150 nm;
2) PrFeO as the carrier3Modified core-shell octahedral structure Fe2O3Preparation of ethyl acetate gas sensor with nano particles as sensitive layer
PrFeO is added3Modified core-shell octahedral structure Fe2O3Putting the nano particles into a mortar, and grinding for 5-10 minutes to uniformly disperse the nano material powder; then, dropping deionized water (the mass ratio of the nano particles to the deionized water is 5: 1-3) into the mortar, and continuously grinding for 5-15 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 PrFeO with the coating thickness of 2-4 mu m3Modified core-shell octahedral structure Fe2O3A nanoparticle sensitive layer; finally, aging for 48-72 hours under the direct current of 80-100 mA in an environment with the relative humidity of 35-50% RH and the temperature of 20-35 ℃, thereby obtaining the PrFeO3Modified core-shell octahedral structure Fe2O3The ethyl acetate gas sensor with the nano particles as the sensitive layer.
After the gas sensor was prepared, the gas-sensitive performance of ethyl acetate was tested (CGS-1 TP type gas-sensitive performance tester, erlite technologies ltd, beijing).
The invention has the advantages and positive effects that: PrFeO prepared by the invention3Modified core-shell octahedral structure Fe2O3The ethyl acetate gas sensor with the nano particles as the sensitive layer has the characteristics of simple preparation method, low cost, high response recovery speed and hopeful large-scale production, and has good detection performance on ethyl acetate gas.
Drawings
FIG. 1 shows PrFeO3Modified core-shell octahedral structure Fe2O3SEM 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 PrFeO3Modified core-shell octahedral structure Fe2O3TEM images of the nanoparticles, corresponding to example 1;
FIG. 4 shows PrFeO3Modified core-shell octahedral structure Fe2O3XRD pattern of nanoparticles, corresponding to example 1;
FIG. 5 is a schematic structural view of an ethyl acetate 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 ethyl acetate gas sensor prepared according to the present invention at a working temperature of 206 ℃ and the ethyl acetate concentration, wherein the responsivity is expressed as 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 the ethyl acetate gas sensor prepared according to the present invention at a working temperature of 206 ℃ and an ethyl acetate concentration of 5ppm, corresponding to example 1;
FIG. 8 is a graph showing the response recovery of the ethyl acetate gas sensor prepared according to the present invention at a working temperature of 206 ℃ and an ethyl acetate concentration of 20ppm, corresponding to example 2;
FIG. 9 is a graph showing the response recovery of the ethyl acetate gas sensor prepared according to the present invention at a working temperature of 206 ℃ and an ethyl acetate concentration of 100ppm, corresponding to example 3;
FIG. 10 is a schematic diagram showing the selective characteristics of the ethyl acetate gas sensor prepared according to the present invention at a working temperature of 206 ℃ and a gas concentration of 100ppm, corresponding to example 1.
PrFeO is seen from FIGS. 1 and 23Modified Fe2O3The nano particles are in a regular core-shell octahedral structure, and the particle size is about 500-700 nm.
From FIG. 3, PrFeO can be seen3Modified core-shell octahedral structure Fe2O3The nano-particles have the characteristic of porous structure, the thickness of a shell layer is about 8-10 nm, and the size of an inner core is about 350-400 nm.
As can be seen from FIG. 4, the XRD spectrum shows PrFeO3And Fe2O3Indicating that the sample comprises PrFeO3And Fe2O3And (4) crystals.
As shown in FIG. 5, the gas sensor is made of Al2O3Substrate 1, Pd metal interdigital electrode 3 and PrFeO3Modified core-shell octahedral structure Fe2O3A nanoparticle sensitive layer 2.
As shown in FIG. 6, when the gas sensor is operated at 206 ℃, the sensitivity of the gas sensor increases with the increase of the concentration of ethyl acetate, and the curve shows a good linear relationship in the concentration range of 1-20 ppm.
As shown in fig. 7, when the gas sensor was operated at 206 c and the ethyl acetate concentration was 5ppm, the response of the gas sensor was about 10s and the recovery time of the gas sensor was about 8 s. Corresponding to example 1.
As shown in fig. 8, when the gas sensor was operated at 206 c and the ethyl acetate concentration was 20ppm, the response of the gas sensor was about 8s and the recovery time of the gas sensor was about 9 s. Corresponding to example 2.
As shown in fig. 9, when the gas sensor was operated at 206 c and the ethyl acetate concentration was 100ppm, the response of the gas sensor was about 11s and the recovery time of the gas sensor was about 8 s. Corresponding to example 3.
As shown in fig. 10, when the gas sensor has an operating temperature of 206 ℃ and a gas concentration of 100ppm, the response of the gas sensor to ethyl acetate is greater than that of other detection gases. The gas sensor showed good selectivity.
Detailed Description
Example 1:
firstly, wiping Al with Pd metal interdigital electrodes with the width of 3mm and the length of 4mm prepared by a screen printing technology by using acetone and ethanol cotton balls respectively2O3Cleaning 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; and 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 degrees and a pressure of 5 newtons, printing and drying the electrodes, and completing the preparation of the Pd metal interdigital electrode after ultraviolet curing, wherein the finger width and the electrode spacing of the Pd metal interdigital electrode are both 0.15mm, and the thickness of the Pd metal interdigital electrode is 100 nm.
Preparing an octahedral organic metal framework nano material MIL-53 by adopting a solvothermal method: under the condition of room temperature, firstly weighing 30mL of dimethylformamide, then adding 0.2g of terephthalic acid and 0.6g of ferric chloride hexahydrate, and stirring for 20 minutes; transferring the mixed solution into a reaction kettle to react for 20 hours at 120 ℃; cooling the obtained product to room temperature, centrifugally cleaning the product by using deionized water, and drying for 24 hours at the temperature of 70 ℃ to obtain an octahedral organic metal framework nano material MIL-53;
PrFeO3and (3) a nanoparticle modification process: adding 0.04g of MIL-53 into 15mL of absolute ethyl alcohol at room temperature, and stirring for 1 hour to uniformly disperse the MIL-53 nano material in the solution; then adding 0.04g of praseodymium nitrate hexahydrate and 0.5g of sodium citrate into the mixed solution, and continuing stirring for 2 hours to make the solution uniform; and finally, centrifugally cleaning the obtained product by using deionized water, drying the product at room temperature, putting the product in a high-temperature tube furnace, vacuumizing the furnace, filling mixed gas (the volume flow ratio of nitrogen to oxygen is 9: 1), and calcining the product at 350 ℃ for 2 hours to obtain 0.008g of PrFeO3Modified core-shell octahedral structure Fe2O3Nanoparticle sensitive layer material.
Based on PrFeO3Modified core-shell octahedral structure Fe2O3Preparing a gas sensor with nano particles as a sensitive layer: drying the PrFeO3Modified core-shell octahedral structure Fe2O3The nano particles are put into a mortar and ground for 5 minutes, and deionized water (PrFeO) is dripped into the mortar3Modified core-shell octahedral structure Fe2O3The mass ratio of the nanoparticles to the water is 5: 2) then, continuously grinding for 5 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 room temperature to obtain PrFeO3Modified core-shell octahedral structure Fe2O3The thickness of the nanoparticle sensitive layer is 2 μm; finally, the prepared gas sensor is aged for 22 hours under the direct current of 100mA in the environment with the relative humidity of 35 percent RH and the temperature of 22 ℃, thereby obtaining the PrFeO of the invention3Modified core-shell octahedral structure Fe2O3The gas sensor takes nano particles as a sensitive layer and metal Pd as an interdigital electrode.
Prepared in the above examples as PrFeO3Modified core-shell octahedral structure Fe2O3The gas sensor with nano particles as a sensitive layer and metal Pd as an interdigital electrode has the gas-sensitive performance thatTested by a CGS-1TP type gas-sensitive performance tester of Elite technologies, Inc. of Beijing. The gas-sensitive performance indexes are as follows:
sensitivity 2.65(5ppm ethyl acetate)
The response time was 10 seconds and the recovery time was 8 seconds.
Example 2
Firstly, wiping Al with Pd metal interdigital electrodes with the width of 3mm and the length of 4mm prepared by a screen printing technology by using acetone and ethanol cotton balls respectively2O3Cleaning 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; and then, injecting the paste onto a silk screen plate with interdigital electrode patterns, scraping the paste under the conditions of an inclination angle of 45 degrees and a pressure of 10 newtons, printing and drying the electrodes, and completing the preparation of the Pd metal interdigital electrode after ultraviolet curing, wherein the finger width and the electrode spacing of the Pd metal interdigital electrode are both 0.20mm, and the thickness of the Pd metal interdigital electrode is 100 nm.
Preparing an octahedral organic metal framework nano material MIL-53 by adopting a solvothermal method: under the condition of room temperature, firstly weighing 30mL of dimethylformamide, then adding 0.2g of terephthalic acid and 0.8g of ferric chloride hexahydrate, and stirring for 30 minutes; the mixed solution was transferred to a reaction vessel and reacted at 120 ℃ for 24 hours. Cooling the obtained product to room temperature, centrifugally cleaning the product by using deionized water, and drying for 24 hours at the temperature of 70 ℃ to obtain an octahedral organic metal framework nano material MIL-53;
PrFeO3and (3) a nanoparticle modification process: adding 0.04g of MIL-53 into 20mL of absolute ethyl alcohol at room temperature, and stirring for 1 hour to uniformly disperse the MIL-53 nano material in the solution; then, 0.08g of praseodymium nitrate hexahydrate and 0.7g of sodium citrate were added to the above mixed solution, and stirring was continued for 2 hoursThe solution is uniform; and finally, centrifugally cleaning the obtained product by using deionized water, drying the product at room temperature, putting the product in a high-temperature tube furnace, vacuumizing the furnace, filling mixed gas (the volume flow ratio of nitrogen to oxygen is 9: 1), and calcining the product at 350 ℃ for 3 hours to obtain 0.008g of PrFeO3Modified core-shell octahedral structure Fe2O3Nanoparticle sensitive layer material.
Based on PrFeO3Modified core-shell octahedral structure Fe2O3Preparing a gas sensor with nano particles as a sensitive layer: drying the PrFeO3Modified core-shell octahedral structure Fe2O3The nano particles are put into a mortar and ground for 5 minutes, and deionized water (PrFeO) is dripped into the mortar3Modified core-shell octahedral structure Fe2O3The mass ratio of the nanoparticles to the water is 5: 2.5), continuously grinding for 5 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 room temperature to obtain PrFeO3Modified core-shell octahedral structure Fe2O3The thickness of the nanoparticle sensitive layer is 3 μm; finally, the prepared gas sensor is aged for 22 hours under the direct current of 100mA in the environment with the relative humidity of 40 percent RH and the temperature of 25 ℃, thereby obtaining the PrFeO of the invention3Modified core-shell octahedral structure Fe2O3The gas sensor takes nano particles as a sensitive layer and metal Pd as an interdigital electrode.
Prepared in the above examples as PrFeO3Modified core-shell octahedral structure Fe2O3The 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 9.57(20ppm ethyl acetate)
The response time was 8 seconds and the recovery time was 9 seconds.
Example 3
Firstly, the cotton balls with acetone and ethanol are respectively used for wiping the silk screen printing beltAl prepared by brush technology and having Pd metal interdigital electrode with width of 3mm and length of 4mm2O3Cleaning 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; and 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 degrees and a pressure of 5 newtons, printing and drying the electrodes, and completing the preparation of the Pd metal interdigital electrode after ultraviolet curing, wherein the finger width and the electrode spacing of the Pd metal interdigital electrode are both 0.20mm, and the thickness of the Pd metal interdigital electrode is 100 nm.
Preparing an octahedral organic metal framework nano material MIL-53 by adopting a solvothermal method: under the condition of room temperature, firstly weighing 50mL of dimethylformamide, then adding 0.4g of terephthalic acid and 0.8g of ferric chloride hexahydrate, and stirring for 20 minutes; the mixed solution was transferred to a reaction vessel and reacted at 120 ℃ for 20 hours. Cooling the obtained product to room temperature, centrifugally cleaning the product by using deionized water, and drying for 24 hours at the temperature of 80 ℃ to obtain an octahedral organic metal framework nano material MIL-53;
PrFeO3and (3) a nanoparticle modification process: adding 0.06g of MIL-53 into 20mL of absolute ethyl alcohol at room temperature, and stirring for 2 hours to uniformly disperse the MIL-53 nano material in the solution; then adding 0.16g of praseodymium nitrate hexahydrate and 0.7g of sodium citrate into the mixed solution, and continuing stirring for 3 hours to make the solution uniform; finally, centrifugally cleaning the obtained product with deionized water, drying at room temperature, placing the obtained product in a high-temperature tube furnace, vacuumizing, filling mixed gas (the volume flow ratio of nitrogen to oxygen is 9: 1.2), and calcining at 400 ℃ for 2 hours to obtain 0.01g of PrFeO3Modified core-shell octahedral structure Fe2O3Nanoparticle sensitive layer material.
Based on PrFeO3Modified core-shell octahedral structure Fe2O3Preparing a gas sensor with nano particles as a sensitive layer: drying the PrFeO3Modified core-shell octahedral structure Fe2O3The nano particles are put into a mortar and ground for 5 minutes, and deionized water (PrFeO) is dripped into the mortar3Modified core-shell octahedral structure Fe2O3The mass ratio of the nanoparticles to the water is 5: 2.5), continuously grinding for 5 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 room temperature to obtain PrFeO3Modified core-shell octahedral structure Fe2O3The thickness of the nanoparticle sensitive layer is 2 μm; finally, the prepared gas sensor is aged for 22 hours under the direct current of 100mA in the environment with the relative humidity of 50 percent RH and the temperature of 28 ℃, thereby obtaining the PrFeO of the invention3Modified core-shell octahedral structure Fe2O3The gas sensor takes nano particles as a sensitive layer and metal Pd as an interdigital electrode.
Prepared in the above examples as PrFeO3Modified core-shell octahedral structure Fe2O3The 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 23.89(100ppm ethyl acetate)
The response time was 11 seconds and the recovery time was 8 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. PrFeO as one new kind of catalyst3Modified core-shell octahedral structure Fe2O3The ethyl acetate gas sensor with the nano particles as the sensitive layer sequentially comprises metal interdigital fingers with Pd from bottom to topAl of electrode2O3Substrate, metal interdigital electrode on Pd and Al2O3The sensitive layer prepared by coating technology on the substrate; the method is characterized in that: with PrFeO3Modified core-shell octahedral structure Fe2O3The nano particles are a sensitive layer, the particle size of the nano particles is 500 nm-700 nm, and a large amount of PrFeO3The nano particles grow on the core-shell octahedral structure Fe2O3On the surface of (a); and PrFeO3Modified core-shell octahedral structure Fe2O3The nano-particle sensitive layer is prepared by the following steps,
preparing an organic metal framework nano material MIL-53 with an octahedral structure: weighing 30-50 mL of dimethylformamide at room temperature, adding 0.2-0.4 g of terephthalic acid and 0.6-0.8 g of ferric chloride hexahydrate, and stirring for 10-30 minutes; transferring the obtained mixed solution into a reaction kettle, reacting at 120-150 ℃ for 20-24 hours, cooling the obtained product to room temperature, centrifugally cleaning the product with deionized water, and drying at 70-80 ℃ for 20-30 hours to obtain an octahedral organic metal framework nano material MIL-53;
②PrFeO3modified core-shell octahedral structure Fe2O3Preparing a nano material: adding the octahedral organic metal framework nano material MIL-53 nano material prepared in the step I into 15-25 mL of absolute ethyl alcohol at room temperature, and stirring for 1-2 hours to uniformly disperse the octahedral organic metal framework nano material MIL-53 in the solution; then adding 0.04-0.16 g of praseodymium nitrate hexahydrate and 0.5-0.7 g of sodium citrate into the mixed solution, and continuing stirring for 2-3 hours to make the solution uniform; and finally, centrifugally cleaning the obtained product by using deionized water, drying the centrifugal product at room temperature, placing the obtained product in a high-temperature tube furnace, vacuumizing, filling mixed gas, and calcining for 2-3 hours at 350-400 ℃ to obtain PrFeO3Modified core-shell octahedral structure Fe2O3A nanoparticle sensitive layer material; the mixed gas is the mixture of nitrogen and oxygen, and the volume flow ratio is 9: 1 to 1.2.
2. The compound of claim 1 as PrFeO3Modified core-shell octahedral structure Fe2O3The ethyl acetate gas sensor with the nano particles as the sensitive layer is characterized in that: the finger width and the finger spacing of the Pd metal interdigital electrode are both 0.15-0.20 mm, and the thickness is 100-150 nm; the thickness of the sensitive layer is 2-4 mu m.
3. A composition of claim 1 as PrFeO3Modified core-shell octahedral structure Fe2O3The preparation method of the ethyl acetate 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 electrodes by using acetone and ethanol 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) with PrFeO3Modified core-shell octahedral structure Fe2O3Preparation of ethyl acetate gas sensor with nano particles as sensitive layer
The prepared PrFeO3Modified core-shell octahedral structure Fe2O3Putting the nano particles into a mortar, and grinding for 20-30 minutes to uniformly disperse the nano material powder; then, dripping deionized water into the mortar, and continuously grinding for 5-15 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 PrFeO with the coating thickness of 2-4 mu m3Modified core-shell octahedral structure Fe2O3A nanoparticle sensitive layer; finally, aging for 48-72 hours under the direct current of 80-100 mA in an environment with the relative humidity of 35-50% RH and the temperature of 20-35 ℃, thereby obtaining the PrFeO3Modified core-shell octahedral structure Fe2O3Ethyl acetate gas with nano-particles as sensitive layerA body sensor.
4. The compound of claim 3 as PrFeO3Modified core-shell octahedral structure Fe2O3The preparation method of the ethyl acetate gas sensor with the nano particles as the sensitive layer is characterized by comprising the following steps: the mass ratio of the nano particles to the deionized water in the step (2) is 5: 1 to 3.
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