CN114076783A - 2-butanone sensor based on ZnO nano sensitive material and preparation method thereof - Google Patents
2-butanone sensor based on ZnO nano sensitive material and preparation method thereof Download PDFInfo
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- CN114076783A CN114076783A CN202111365331.1A CN202111365331A CN114076783A CN 114076783 A CN114076783 A CN 114076783A CN 202111365331 A CN202111365331 A CN 202111365331A CN 114076783 A CN114076783 A CN 114076783A
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- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
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Abstract
The invention relates to a 2-butanone sensor based on a ZnO nano sensitive material and a preparation method thereof, belonging to the technical field of semiconductor oxide gas sensors. Al with two parallel, annular and mutually separated gold electrodes on the outer surface2O3Ceramic tube substrate coated with Al2O3APTES functionalized ZnO nano sensitive material on the outer surface of the ceramic tube and the gold electrode, Al2O3A nickel-cadmium heating coil in the ceramic tube; 2-methylimidazole zinc salt is selected as a self-sacrifice template, a porous ZnO nano material is obtained through high-temperature calcination, 3-aminopropyltriethoxysilane is modified on the surface of the ZnO nano material, the interaction between 2-butanone and a sensitive material is increased, and the response of the sensor to 2-butanone is remarkably improved. The device has novel structure and small volume, is suitable for mass production, and has wide application prospect in the sensor based on the APTES functionalized ZnO nano material.
Description
Technical Field
The invention belongs to the technical field of semiconductor oxide gas sensors, and particularly relates to a 2-butanone sensor based on a ZnO nano sensitive material and a preparation method thereof.
Background
The development of science and technology makes people's life more convenient. Meanwhile, some toxic Volatile Organic Compounds (VOCs) are generated, and the environmental safety of our life and work is seriously threatened. 2-butanone is a colorless volatile organic compound with a slightly pungent smell, and has been widely used in the living fields of plastics, coatings, medicines, textiles, foods, artificial leather, cosmetics, electronic products and the like. Short term inhalation or exposure to 2-butanone can irritate the eyes, nose and respiratory system of the human body, and excessive exposure to 2-butanone can inhibit the central system, leading to coma and death. Therefore, the development of a sensor which is simple to manufacture, low in cost and capable of rapidly detecting 2-butanone is an important measure for ensuring environmental safety and avoiding potential hazards.
The metal oxide semiconductor gas sensor has the advantages of low cost, simple preparation, high sensitivity, quick response/recovery and the like, and plays an important role in the fields of industry, agriculture, environmental protection, medical treatment and the like. ZnO is an important and common N-type metal oxide semiconductor with a high share in the semiconductor-type gas sensor market. At present, researchers have successfully synthesized ZnO with various nano structures, such as nanowires, nanorods, nanorings, nanosheets, three-dimensional layered structures and the like, for detecting toxic and harmful gases. However, the existing ZnO-based gas sensors cannot achieve high-sensitivity and high-selectivity detection of low-concentration, particularly 2-butanone below the ppm level. In recent years, researchers find that modifying an organic monolayer on the surface of a semiconductor oxide is a tool for constructing a high-efficiency sensor, but the target gas for the method is limited to NH at present3And NO2The targeted detection of the 2-butanone by retrieval is not reported, so that the improvement of the performance of the ZnO-based gas sensor by using the modification of the organic monomolecular layer has important scientific and practical significance.
Disclosure of Invention
The invention provides a ZnO nano sensitive material-based 2-butanone sensor and a preparation method thereof, which aim to solve the problem that the existing ZnO-based gas sensor cannot realize high-sensitivity and high-selectivity detection of low-concentration 2-butanone.
The invention adopts the technical scheme that the Al with two parallel, annular and mutually separated gold electrodes on the outer surface2O3Ceramic tube substrate coated with Al2O3Nano sensitive material on the outer surface of ceramic tube and gold electrode, Al2O3A nickel-cadmium heating coil in the ceramic tube; the nano sensitive material is a ZnO nano material modified by 3-aminopropyl triethoxysilane (APTES), and the preparation steps are as follows:
adding 3-5 mmol of zinc nitrate into 30-40 mL of ethanol, and uniformly stirring to obtain a solution A;
adding 15-16 mmol of 2-methylimidazole into 30-40 mL of ethanol, and uniformly stirring to form a solution B;
pouring the solution B into the solution A, and continuing stirring and aging;
fourthly, centrifuging, washing and drying the product obtained in the step three to obtain a 2-methylimidazole zinc salt ZIF-8 sample;
fifthly, sintering the ZIF-8 sample obtained in the step four at 500-600 ℃ to obtain a ZnO nano material;
sixthly, adding the ZnO sample obtained in the step of the.
In the step (3), the stirring time is 20-30 minutes, and the aging time is 22-24 hours.
Drying at 70-90 ℃ in the step (4).
Sintering for 1-3 hours in the step (5) of the invention.
In the ethanol solution containing APTES in step (6) of the present invention, VAPTES：VEthanol＝0.2％～1％。
A preparation method of a 2-butanone sensor based on a ZnO nano sensitive material comprises the following steps:
a method for functionalizing an APTESThe ZnO nano sensitive material is dispersed in a proper amount of deionized water to form pasty slurry, and then a small amount of slurry is dipped and evenly coated on the outer surface of the Al nano sensitive material which is provided with two parallel, annular and mutually separated gold electrodes2O3Forming a sensitive material film on the surface of the ceramic tube, and enabling the sensitive material to completely cover the annular gold electrode;
baking the sensitive material at 50-100 ℃ for 30-45 minutes, and drying the sensitive material, then, adding Al2O3Sintering the ceramic tube at 250-300 ℃ for 2-3 hours; then passing a nickel-cadmium heating coil through the Al2O3And (3) taking the inside of the ceramic tube as a heating wire, and finally welding and packaging the device to obtain the 2-butanone sensor based on the ZnO nano sensitive material.
The thickness of the sensitive material film formed in the step (1) is 10-30 mu m.
The resistance value of the nickel-cadmium heating coil in the step (2) is 30-40 omega.
Al according to the invention2O3The ceramic tube has a length of 4-4.5 mm, an outer diameter of 1.2-1.5 mm and an inner diameter of 0.8-1.0 mm; the distance between the Au electrodes is 0.5-0.6 mm, and the width of the Au electrodes is 0.4-0.5 mm.
The invention adopts a sensitization method of organic monomolecular layer functionalized semiconductor oxide, and improves the sensitivity of the ZnO-based sensor to 2-butanone through modification of 3-Aminopropyltriethoxysilane (APTES). The ZnO modified by APTES has a wider electron depletion layer, which increases the capability of a sensitive material to accept electrons from 2-butanone. Furthermore, the nucleophilic-NH with negative charge on the APTES monomolecular layer2Nucleophilic addition reaction with electrophilic carbon atom of carbon heteroatom double bond (C ═ O) on 2-butanone molecule can promote interaction of 2-butanone and sensitive material. Finally, the sensitivity of the ZnO-based sensor to the 2-butanone is improved.
The 2-butanone sensor based on the ZnO nano sensitive material prepared by the invention has the following advantages:
the synthesis method of the APTES functionalized ZnO nano sensitive material is simple and has low cost.
The introduction of APTES increases the interaction between 2-butanone and sensitive materials, so that the response of the sensor to the 2-butanone is obviously improved, and an effective method is provided for improving the sensitivity of the semiconductor oxide type sensor to low-concentration 2-butanone.
3. The sensor with the commercially available tubular structure is adopted, the device process is simple, the size is small, and the sensor is suitable for industrial mass production, so that the sensor has important application value.
Drawings
FIG. 1 is a schematic structural view of a ZnO-based 2-butanone sensor according to the present invention;
FIG. 2 is XRD patterns of ZnO prepared in comparative example 1 and APTES functionalized ZnO nano-sensitive material prepared in example 1;
FIG. 3 is TEM images (a-b) and HRTEM images (c) of ZnO prepared in comparative example 1, TEM images (d-e), HRTEM images (f) and element distribution spectra (g-k) of APTES/ZnO prepared in example 1;
FIG. 4 is a graph showing the sensitivity of the sensors prepared in comparative example 1 and example 1 to 50ppm 2-butanone at a working temperature range of 150 to 300 ℃;
FIG. 5 is a graph showing the dynamic response of the sensors prepared in comparative example 1 and example 1 to 50ppm 2-butanone at an operating temperature of 260 ℃;
FIG. 6 is a graph showing the selectivity of the sensors prepared in comparative example 1 and example 1 for 50ppm of various gases at a working temperature of 260 ℃.
Detailed Description
As shown in FIG. 1, the ZnO-based 2-butanone sensor of the following example consists of Al with two parallel, annular and mutually separated gold electrodes 2 on the outer surface2O3 Ceramic tube 1 substrate, coating Al2O3The nano sensitive material 5 on the outer surface of the ceramic tube and the gold electrode is arranged on the Al2O3A nickel-cadmium heating coil 4 in the ceramic tube, and a platinum wire 3 connected with the annular gold electrode 2.
Example 1
1. Adding 4mmol of zinc nitrate into 40mL of ethanol, and uniformly stirring to obtain a solution A;
2. adding 16mmol of 2-methylimidazole into 40mL of ethanol under strong stirring to form a solution B; then, the process of the present invention is carried out,
3. pouring the solution B into the solution A, continuously stirring for 30 minutes and aging for 24 hours;
4. centrifuging the product obtained in the step three, washing the product with ethanol for several times, and drying the product at 80 ℃ to obtain a 2-methylimidazolium zinc salt ZIF-8 sample;
5. sintering a ZIF-8 sample at 550 ℃ for 2 hours to obtain a ZnO nano material;
6. 100mg of ZnO sample was added to the ethanol solution containing APTES, VAPTES：VEthanolStirring for 6h, washing with ethanol for three times, and drying at 70 ℃ to obtain an APTES functionalized ZnO sensitive nano material marked as 0.5 vol% APTES/ZnO;
7. 50mg of APTES functionalized ZnO nano sensitive material is dispersed in 0.3mL of deionized water to form pasty slurry, a small amount of slurry is dipped by a small brush and evenly coated on Al of which the outer surface is provided with two parallel, annular and mutually separated gold electrodes2O3Forming a sensitive material film with the thickness of 30 mu m on the surface of the ceramic tube, and enabling the sensitive material to completely cover the annular gold electrode;
8. baking at 75 deg.C for 30 min, drying the sensitive material, and adding Al2O3The ceramic tube was sintered at 300 ℃ for 2 hours, and then a nickel-cadmium heating coil having a resistance value of 30 Ω was passed through Al2O3And finally, welding and packaging the device according to a general indirectly heated gas sensitive element to obtain the ethanol sensor based on the APTES functionalized ZnO nano sensitive material.
Example 2
1. Adding 3mmol of zinc nitrate into 30mL of ethanol, and uniformly stirring to obtain a solution A;
2. adding 15mmol of 2-methylimidazole into 30mL of ethanol under strong stirring to form a solution B; then, the process of the present invention is carried out,
3. pouring the solution B into the solution A, continuously stirring for 20 minutes and aging for 22 hours;
4. centrifuging the product obtained in the step three, washing the product with ethanol for several times, and drying the product at 70 ℃ to obtain a 2-methylimidazolium zinc salt ZIF-8 sample;
5. sintering a ZIF-8 sample at 500 ℃ for 1 hour to obtain a ZnO nano material;
6. 100mg of ZnO sample was added to the ethanol solution containing APTES, VAPTES：VEthanolStirring for 5h, washing with ethanol for three times, and drying at 75 ℃ to obtain an APTES functionalized ZnO sensitive nano material marked as 0.2 vol% APTES/ZnO;
7. 50mg of APTES functionalized ZnO nano sensitive material is dispersed in 0.3mL of deionized water to form pasty slurry, a small amount of slurry is dipped by a small brush and evenly coated on Al of which the outer surface is provided with two parallel, annular and mutually separated gold electrodes2O3Forming a sensitive material film with the thickness of 10 mu m on the surface of the ceramic tube, and enabling the sensitive material to completely cover the annular gold electrode;
8. baking at 50 deg.C for 40 min, drying the sensitive material, and adding Al2O3The ceramic tube was sintered at 250 ℃ for 2.5 hours, and then a nickel cadmium heating coil having a resistance value of 35 Ω was passed through Al2O3And finally, welding and packaging the device according to a general indirectly heated gas sensitive element to obtain the ethanol sensor based on the APTES functionalized ZnO nano sensitive material.
Example 3
1. Adding 5mmol of zinc nitrate into 35mL of ethanol, and uniformly stirring to obtain a solution A;
2. adding 15.5mmol of 2-methylimidazole into 35mL of ethanol under strong stirring to form a solution B; then, 3, pouring the solution B into the solution A, continuing stirring for 25 minutes and aging for 23 hours;
4. centrifuging the product obtained in the step three, washing the product with ethanol for several times, and drying the product at 90 ℃ to obtain a 2-methylimidazolium zinc salt ZIF-8 sample;
5. sintering a ZIF-8 sample at 600 ℃ for 3 hours to obtain a ZnO nano material;
6. 100mg of ZnO sample was added to the ethanol solution containing APTES, VAPTES：VEthanolStirring for 5.5h, washing with ethanol three times, and drying at 90 deg.C to obtainThe APTES functionalized ZnO sensitive nano material is marked as 1 vol% APTES/ZnO;
7. 50mg of APTES functionalized ZnO nano sensitive material is dispersed in 0.3mL of deionized water to form pasty slurry, a small amount of slurry is dipped by a small brush and evenly coated on Al of which the outer surface is provided with two parallel, annular and mutually separated gold electrodes2O3Forming a sensitive material film with the thickness of 20 microns on the surface of the ceramic tube, and enabling the sensitive material to completely cover the annular gold electrode;
8. baking at 100 deg.C for 45 min, drying the sensitive material, and adding Al2O3The ceramic tube was sintered at 280 ℃ for 3 hours, and then a nickel-cadmium heating coil having a resistance value of 40 Ω was passed through Al2O3And finally, welding and packaging the device according to a general indirectly heated gas sensitive element to obtain the ethanol sensor based on the APTES functionalized ZnO nano sensitive material.
The effect of the present invention is further illustrated below by comparing the comparative example with example 1 of the present invention.
Comparative example
1. Adding 4mmol of zinc nitrate into 40mL of ethanol, and uniformly stirring to obtain a solution A; 16mmol of 2-methylimidazole was added to 40mL of ethanol under vigorous stirring to form a solution B, and then the solution B was poured into the solution A, stirred for 30 minutes and aged for 24 hours, and then the product was washed with ethanol several times and dried at 80 ℃ to obtain a sample of 2-methylimidazole zinc salt (ZIF-8). Finally, sintering the ZIF-8 sample at 550 ℃ for 2 hours to obtain a ZnO nano material;
2. 50mg of ZnO nano sensitive material is dispersed in 1mL of deionized water to form pasty slurry, a small amount of slurry is dipped by a small brush and evenly coated on the outer surface of Al with two parallel, annular and mutually separated gold electrodes2O3Forming a sensitive material film with the thickness of 30 mu m on the surface of the ceramic tube, and enabling the sensitive material to completely cover the annular gold electrode;
3. baking under infrared lamp for 30 min, drying the sensitive material, and adding Al2O3The ceramic tube is sintered for 2 hours at 300 DEG CThen, a nickel-cadmium heating coil having a resistance value of 30 Ω was passed through Al2O3And finally, welding and packaging the device according to a general indirectly heated gas sensitive element to obtain the 2-butanone sensor based on the ZnO nano sensitive material.
Al2O3The ceramic tube has a length of 4-4.5 mm, an outer diameter of 1.2-1.5 mm and an inner diameter of 0.8-1.0 mm; the distance between the Au electrodes is 0.5-0.6 mm, and the width of the Au electrodes is 0.4-0.5 mm.
As shown in fig. 2, all diffraction peaks of both samples could be well classified as the rutile structure of ZnO, which is in full agreement with the standard card (JCPDS 36-1451), and APTES functionalization did not have an effect on the crystalline structure of the ZnO material.
As shown in FIG. 3, after the ZnO is modified by the APTES, the shape of the sensitive material is not obviously changed, and the distribution of Zn, O, N and Si is consistent with the position of the APTES/ZnO particles, which shows that the APTES is uniformly distributed on the surface of the ZnO particles.
As shown in fig. 4, the sensitivity of the sensor is greatly affected by the operating temperature, and in this operation, 260 ℃ is the optimum operating temperature of the sensor.
As shown in FIG. 5, the sensor has a fast response recovery rate when detecting 2-butanone, and it is noted that the sensor resistance significantly increases after modification with APTES, which is mainly caused by the extraction of electrons from the conduction band of ZnO by APTES.
As shown in fig. 6, the selectivity of the sensor for 2-butanone in example 1 was significantly improved as compared with the comparative example. The sensitivity of the sensor to 2-butanone was highest among all the VOC gases tested.
Note: for reducing gases, the response (sensitivity) of the sensor to the gas to be measured is defined as S ═ Ra/Rg, where Ra and Rg represent the resistance values of the sensor in air and in the target gas, respectively, and the response time and recovery time are defined as the time required for the resistance value of the sensor to reach 90% of the total resistance change from a stable value during adsorption or desorption, respectively.
Claims (9)
1. ZnO-based nano sensitive materialA2-butanone sensor is composed of Al with two parallel, annular and separated gold electrodes on its external surface2O3Ceramic tube substrate coated with Al2O3Nano sensitive material on the outer surface of ceramic tube and gold electrode, Al2O3A nickel-cadmium heating coil in the ceramic tube; the method is characterized in that: the nano sensitive material is a ZnO nano material modified by 3-aminopropyl triethoxysilane (APTES), and the preparation steps are as follows:
(1) adding 3-5 mmol of zinc nitrate into 30-40 mL of ethanol, and uniformly stirring to obtain a solution A;
(2) adding 15-16 mmol of 2-methylimidazole into 30-40 mL of ethanol, and uniformly stirring to form a solution B;
(3) pouring the solution B into the solution A, and continuing stirring and aging;
(4) centrifuging, washing and drying the product obtained in the step three to obtain a 2-methylimidazole zinc salt ZIF-8 sample;
(5) sintering the ZIF-8 sample obtained in the fourth step at 500-600 ℃ to obtain a ZnO nano material;
(6) and fifthly, adding the ZnO sample obtained in the step into an ethanol solution containing APTES, stirring for 5-6 hours, washing with ethanol, and drying at 70-90 ℃ to obtain the APTES modified ZnO sensitive nano material.
2. The 2-butanone sensor based on the ZnO nano-sensitive material as claimed in claim 1, wherein: in the step (3), the stirring time is 20-30 minutes, and the aging time is 22-24 hours.
3. The 2-butanone sensor based on the ZnO nano-sensitive material as claimed in claim 1, wherein: and (4) drying at 70-90 ℃.
4. The 2-butanone sensor based on the ZnO nano-sensitive material as claimed in claim 1, wherein: and (5) sintering for 1-3 hours.
5. The 2-butanone sensor based on the ZnO nano-sensitive material as claimed in claim 1, wherein: in the ethanol solution containing APTES in the step (6), VAPTES：VEthanol＝0.2％～1％。
6. The preparation method of the ZnO nano sensitive material-based 2-butanone sensor as claimed in any one of claims 1 to 5, comprising the following steps:
(1) dispersing the APTES functionalized ZnO nano-sensitive material in a proper amount of deionized water to form pasty slurry, and then dipping a small amount of slurry to uniformly coat the slurry on Al of which the outer surface is provided with two parallel, annular and mutually separated gold electrodes2O3Forming a sensitive material film on the surface of the ceramic tube, and enabling the sensitive material to completely cover the annular gold electrode;
(2) baking at 50-100 ℃ for 30-45 minutes, and drying the sensitive material, and then adding Al2O3Sintering the ceramic tube at 250-300 ℃ for 2-3 hours; then passing a nickel-cadmium heating coil through the Al2O3And (3) taking the inside of the ceramic tube as a heating wire, and finally welding and packaging the device to obtain the 2-butanone sensor based on the ZnO nano sensitive material.
7. The preparation method of the ZnO nano-sensitive material-based 2-butanone sensor according to claim 6, characterized in that: the thickness of the sensitive material film formed in the step (1) is 10-30 mu m.
8. The preparation method of the ZnO nano-sensitive material-based 2-butanone sensor according to claim 6, characterized in that: and (3) the resistance value of the nickel-cadmium heating coil in the step (2) is 30-40 omega.
9. The preparation method of the ZnO nano-sensitive material-based 2-butanone sensor according to claim 6, characterized in that: al (Al)2O3The ceramic tube has a length of 4-4.5 mm, an outer diameter of 1.2-1.5 mm and an inner diameter of 0.8-1.0 mm; au capacitorThe distance between the electrodes is 0.5-0.6 mm, and the width of the Au electrode is 0.4-0.5 mm.
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