CN112730531B - Preparation method of hydrogen sulfide gas sensor based on molybdenum trioxide nanosheets - Google Patents
Preparation method of hydrogen sulfide gas sensor based on molybdenum trioxide nanosheets Download PDFInfo
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- CN112730531B CN112730531B CN202011556781.4A CN202011556781A CN112730531B CN 112730531 B CN112730531 B CN 112730531B CN 202011556781 A CN202011556781 A CN 202011556781A CN 112730531 B CN112730531 B CN 112730531B
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- G—PHYSICS
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
Abstract
The invention relates to the field of hydrogen sulfide gas sensors, in particular to a preparation method of a hydrogen sulfide gas sensor based on molybdenum trioxide nanosheets. The technical scheme is as follows: in the sensor, molybdenum trioxide nanosheet powder is dispersed in deionized water or ethanol to form a suspension, and then the suspension is uniformly coated on a gold interdigital electrode and heated at the temperature of not more than 150 ℃ to form a thin film; the working temperature of the sensor is within the range of 200-350 ℃; the real-time monitoring signal of the sensor is the change of the resistance value of the sensor under the direct-current voltage of 1V. The invention has the following effects and benefits: compared with the reported hydrogen sulfide gas sensor, the gas sensor using the molybdenum trioxide nanosheet material has better selectivity, high sensitivity and simple preparation.
Description
Technical Field
The invention belongs to the field of hydrogen sulfide gas sensors, and particularly relates to a preparation method of a molybdenum trioxide nanosheet sensitive material and a preparation method of a sensor.
Background
It is known that a certain amount of H2S may cause serious harm to human body and even threaten life. According to the national occupational health Standard of the people' S republic of China (GBZ 2.1-2007) workplace hazardous elements occupational contact Limit chemical hazardous elements, the maximum allowable concentration of H2S is 10mg/m3 (about 7.2 ppm) within one working day. When the H2S concentration is higher than 250ppm, death may result. Therefore, it is of great significance to develop a reliable and efficient H2S gas sensor. Molybdenum trioxide is an important n-type semiconductor, has an energy band gap of about 2.39-2.9eV, and has unique gas-sensitive characteristics. Nanostructured molybdenum trioxide is widely recognized as a viable gas sensor, such as nanorods, nanobelts, nanomembranes, hollow spheres, and the like. However, the development of high performance gas sensors based on nano molybdenum trioxide remains a challenge. There are currently two common strategies to improve the performance of gas sensors: a method for improving the performance of a gas sensor is to load noble metals such as silver, platinum, gold and the like on the surface of a sensitive material; another approach is to control the growth of nanomaterials by specially designed sizes, shapes and morphologies, since the properties of gas sensors are highly dependent on their specific surface area. Among various complicated nanostructures, two-dimensional nanostructures such as nanosheets can be effective as a building block for constructing a crystal-oriented nanodevice due to their anisotropic structure.
Disclosure of Invention
The invention aims to provide a preparation method of a hydrogen sulfide gas sensor based on a molybdenum trioxide nanosheet material, which aims to solve the technical problem that a liquid phase stripping method is utilized to strip bulk molybdenum trioxide into nanosheets, and the characteristics of large specific surface area and many surface active sites are utilized, so that better gas-sensitive response of the hydrogen sulfide gas is obtained.
The technical scheme is as follows:
a preparation method of a hydrogen sulfide gas sensor based on molybdenum trioxide nanosheets is characterized by comprising the following steps:
s1, dispersing molybdenum trioxide nanosheet powder in deionized water or ethanol to form a suspension;
s2, uniformly coating the suspension on a gold interdigital electrode and heating at a temperature not higher than 150 ℃ to form a film; the working temperature of the sensor is within the range of 200-350 ℃, and the real-time monitoring signal of the sensor is under 1V direct-current voltage.
Further, the bulk molybdenum trioxide is stripped into nanosheets by a liquid phase stripping method, and then collected by centrifugal separation and lyophilized.
Further, the preparation method of the nano-scale trioxide comprises the following steps:
d1, mixing and grinding molybdenum trioxide and acetonitrile at a molar ratio of less than or equal to 3;
d2, putting the fully ground powder into ethanol/water or isopropanol/water solution with volume fraction, and carrying out ultrasonic treatment for 1-4 hours by using an ultrasonic processor;
d3, centrifuging at low speed at room temperature to separate large-particle molybdenum trioxide;
d4, collecting a yellow blue supernatant containing the high-concentration molybdenum trioxide nanosheets, and centrifuging at a high speed for a sufficient time to separate the molybdenum trioxide nanosheets;
and D5, collecting the blue precipitate, and freeze-drying by using a freeze dryer to obtain molybdenum trioxide nanosheet powder.
The beneficial effects of the invention are:
the sensor prepared by the preparation method of the hydrogen sulfide gas sensor based on the molybdenum trioxide nanosheets has the characteristics of large surface area and many surface active sites, so that better gas-sensitive response of the hydrogen sulfide gas is obtained; compared with the existing molybdenum trioxide hydrogen sulfide gas sensor, the gas sensor using the molybdenum trioxide nanosheet material has better selectivity, good repeatability and simple preparation.
Drawings
FIG. 1 is an X-ray diffraction pattern of a prepared molybdenum trioxide nanosheet;
FIG. 2 is a transmission electron micrograph of the prepared molybdenum trioxide nanosheets;
FIG. 3 is a real diagram of a gold interdigital electrode;
FIG. 4 is a graph of the change in resistance of the sensor to hydrogen sulfide gas at 300 deg.C;
FIG. 5 is a graph of the change in resistance of the sensor at 300 deg.C for various concentrations of hydrogen sulfide gas;
fig. 6 is a graph comparing the response of a sensor to a common VOC gas at 300 c.
Detailed Description
The preparation method of the hydrogen sulfide gas sensor based on the molybdenum trioxide nanosheets is further described with reference to the accompanying drawings 1-6.
Example 1
A preparation method of a hydrogen sulfide gas sensor based on molybdenum trioxide nanosheets is characterized by comprising the following steps:
s1, dispersing molybdenum trioxide nanosheet powder in deionized water or ethanol to form a suspension;
s2, uniformly coating the suspension on a gold interdigital electrode and heating at a temperature not higher than 150 ℃ to form a film; the working temperature of the sensor is within the range of 200-350 ℃, and the real-time monitoring signal of the sensor is under the direct-current voltage of 1V.
Further, the bulk molybdenum trioxide is stripped into nanosheets by a liquid phase stripping method, and then collected by centrifugal separation and lyophilized.
Further, the preparation method of the nano-oxide sheet comprises the following steps:
d1, mixing and grinding molybdenum trioxide and acetonitrile at a molar ratio of 3;
d2, putting the fully ground powder into ethanol/water or isopropanol/water solution with volume fraction, and carrying out ultrasonic treatment for 1-4 hours by using an ultrasonic processor;
d3, centrifuging at low speed at room temperature to separate large-particle molybdenum trioxide;
d4, collecting a yellowish blue supernatant containing high-concentration molybdenum trioxide nano sheets, wherein the concentration is more than 1mg/ml; centrifuging at high speed for a long enough time to separate molybdenum trioxide nanosheets, wherein the rotating speed is more than 8000rpm;
and D5, collecting the blue precipitate, and freeze-drying by using a freeze dryer to obtain molybdenum trioxide nanosheet powder.
The technical scheme of the invention is that firstly, a liquid phase stripping method is utilized to strip the bulk molybdenum trioxide material into nanosheets. Typical XRD and surface micro-topography characteristics of the prepared nanosheets are shown in figures 1 and 2, respectively. And finally, coating the nano-sheet material on a gold interdigital electrode to obtain the final molybdenum trioxide nano-sheet sensor shown in the attached figure 3.
Example 2
Preparing a nano sheet material of the trioxide: molybdenum trioxide was mixed and milled with acetonitrile in a molar ratio of 3. The fully ground powder is put into ethanol/water or isopropanol/water solution with volume fraction, and is treated by ultrasonic for 1-4 hours by an ultrasonic processor, and then is centrifuged at low speed at room temperature to separate out large-particle molybdenum trioxide. And collecting the yellow blue supernatant containing the high-concentration molybdenum trioxide nanosheets, and centrifuging at high speed for a sufficient time to separate the molybdenum trioxide nanosheets. Collecting blue precipitate, and freeze-drying by using a freeze dryer to obtain molybdenum trioxide nanosheet powder.
Preparing a sensor: molybdenum trioxide nanosheet powder is dispersed in deionized water, ethanol or isopropanol to form a suspension, and the suspension is uniformly coated on a gold interdigital electrode of an alumina ceramic substrate shown in figure 3. The electrode is then heated at a temperature not exceeding 150 c for a period of time to evaporate the water and form a film.
And (3) testing of the sensor: the prepared sensor is placed in a flowing air atmosphere, the sensor is heated to the working temperature range of 200-350 ℃, and then target gas is introduced. The 1V DC voltage is provided by a digital source meter and the resistance change is measured. FIG. 4 shows the resistance change (i.e., the sensing signal) of a typical fabricated sensor under an atmosphere of about 10ppm hydrogen sulfide. After 20 minutes from the sensor, the sensor resistance changed by about 75%. Fig. 5 shows the resistance change (i.e., sensing signal) of a typical prepared sensor under hydrogen sulfide atmosphere with different concentrations. The sensor still responds significantly to a concentration of 0.5ppm hydrogen sulfide gas. Figure 6 shows the response of a typical prepared sensor to 10ppm of different gases. Compared with the reported hydrogen sulfide sensor, the sensor has better gas sensitivity selectivity.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (1)
1. A preparation method of a hydrogen sulfide gas sensor based on molybdenum trioxide nanosheets is characterized by comprising the following steps:
s1, dispersing molybdenum trioxide nanosheet powder in deionized water or ethanol to form a suspension;
s2, uniformly coating the suspension on a gold interdigital electrode and heating at a temperature not higher than 150 ℃ to form a film; the working temperature of the sensor is within the range of 200-350 ℃, and the real-time monitoring signal of the sensor is under the direct-current voltage of 1V;
stripping the block molybdenum trioxide into nanosheets by using a liquid phase stripping method, and then performing centrifugal separation, collection and freeze-drying;
the preparation method of the molybdenum trioxide nanosheet comprises the following steps:
d1, mixing and grinding molybdenum trioxide and acetonitrile in a molar ratio of less than or equal to 3;
d2, putting the fully ground powder into ethanol/water or isopropanol/water solution with volume fraction, and carrying out ultrasonic treatment for 1-4 hours by using an ultrasonic processor;
d3, centrifuging at low speed at room temperature to separate large-particle molybdenum trioxide;
d4, collecting a yellow blue supernatant containing the high-concentration molybdenum trioxide nanosheets, and centrifuging at a high speed for a sufficient time to separate the molybdenum trioxide nanosheets;
and D5, collecting the blue precipitate, and freeze-drying by using a freeze dryer to obtain molybdenum trioxide nanosheet powder.
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| CN113433175B (en) * | 2021-07-05 | 2022-04-05 | 吉林大学 | Resistance type organophosphorus compound sensor based on nitrogen-doped molybdenum trioxide, preparation method and application thereof |
| CN114620767B (en) * | 2022-03-15 | 2024-03-19 | 宁波磁性材料应用技术创新中心有限公司 | Sensitization treatment method of molybdenum oxide nanosheets and resistance type hydrogen sulfide gas sensor |
| CN114988460B (en) * | 2022-07-06 | 2024-02-13 | 重庆大学 | Indium oxide nano material and application thereof |
| CN115159587A (en) * | 2022-07-21 | 2022-10-11 | 江苏先丰纳米材料科技有限公司 | Preparation method of molybdenum trioxide nanosheet loaded ferroferric oxide magnetic nanoparticle |
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