CN114620767B - Sensitization treatment method of molybdenum oxide nanosheets and resistance type hydrogen sulfide gas sensor - Google Patents
Sensitization treatment method of molybdenum oxide nanosheets and resistance type hydrogen sulfide gas sensor Download PDFInfo
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- CN114620767B CN114620767B CN202210251087.4A CN202210251087A CN114620767B CN 114620767 B CN114620767 B CN 114620767B CN 202210251087 A CN202210251087 A CN 202210251087A CN 114620767 B CN114620767 B CN 114620767B
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- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 229910000037 hydrogen sulfide Inorganic materials 0.000 title claims abstract description 87
- 239000007789 gas Substances 0.000 title claims abstract description 80
- 229910000476 molybdenum oxide Inorganic materials 0.000 title claims abstract description 48
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000002135 nanosheet Substances 0.000 title claims abstract description 21
- 206010070834 Sensitisation Diseases 0.000 title abstract description 6
- 230000008313 sensitization Effects 0.000 title abstract description 6
- 230000004044 response Effects 0.000 claims abstract description 35
- 239000000725 suspension Substances 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 10
- 230000005855 radiation Effects 0.000 claims abstract description 9
- 230000035945 sensitivity Effects 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000002002 slurry Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000001514 detection method Methods 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000011084 recovery Methods 0.000 abstract description 5
- 239000002086 nanomaterial Substances 0.000 description 13
- 238000012512 characterization method Methods 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 5
- 229910052750 molybdenum Inorganic materials 0.000 description 5
- 239000011733 molybdenum Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 230000001678 irradiating effect Effects 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000007792 addition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 210000001508 eye Anatomy 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005486 sulfidation Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- 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 provides a sensitization treatment method of molybdenum oxide nano-sheets and a resistance type hydrogen sulfide gas sensor, wherein the molybdenum oxide nano-sheets MoO 3 The molybdenum oxide powder obtained by mixing the molybdenum oxide powder with a solvent to form a suspension, then carrying out ultraviolet radiation, and then drying to evaporate the solvent can effectively improve the sensitivity to hydrogen sulfide, and the resistance response to 50ppb hydrogen sulfide gas is more than 1 when the molybdenum oxide powder is used for a hydrogen sulfide gas sensor. In addition, the resistance response and the resistance recovery performance can be considered by adjusting the ultraviolet irradiation time and the working temperature of the sensor, and the method has good application prospect.
Description
Technical Field
The invention belongs to the technical field of gas sensitive materials and gas sensors, and particularly relates to a sensitization treatment method of molybdenum oxide nanosheets and a resistance type hydrogen sulfide gas sensor.
Background
Hydrogen sulfide is a toxic and hazardous gas that can be mixed with air to form an explosive mixture. Inhalation of small amounts of high concentration hydrogen sulfide by the human body can be fatal in a short period of time, and low concentration hydrogen sulfide has an effect on the eyes, respiratory system and central nervous system. According to the national standard malodorous pollutant emission Standard (GB 14554-1993), the primary emission Standard of Hydrogen sulfide is 0.03mg/m 3 (20 ppb) thus monitoring of hydrogen sulfide gas with a sensorIs very important.
Metal oxide based sensors are widely used for gas detection and monitoring. However, the metal oxide gas sensor has the problems of easy humidity interference, low selectivity, low sensitivity to hydrogen sulfide and the like, and further application of the sensor is hindered.
The literature Bao, j., z.zhang, and y.zheng, H2S sensor based on two-dimensional MoO3 nanofarakes: transition between sulfidation and oxidation, sensors and detectors B: chemical,2021.345: p.130408, reports a hydrogen sulfide sensor based on molybdenum oxide nanoplatelets that has a high selectivity for hydrogen sulfide and is insensitive to environmental humidity changes, but has a low sensitivity for hydrogen sulfide, a minimum detection limit of 500ppb, an order of magnitude different from the national standard concentration requirements.
Disclosure of Invention
Aiming at the state of the art, the invention provides a sensitization treatment method of molybdenum oxide nano-sheets, and the molybdenum oxide nano-sheets treated by the method can effectively improve the sensitivity to hydrogen sulfide and can be used for hydrogen sulfide gas sensors.
The technical scheme provided by the invention is as follows: a sensitization treatment method of molybdenum oxide nanosheets is characterized by comprising the following steps: the molecular formula of the molybdenum oxide nano-sheet is MoO 3 The method comprises the following steps:
(1) Mixing molybdenum oxide nano-sheets with a solvent to form a suspension;
(2) Subjecting the suspension to ultraviolet radiation;
(3) Drying the irradiated suspension to evaporate the solvent and obtain molybdenum oxide powder.
In the step (1), the solvent is not limited, and may include one or two of water, ethanol, and the like. Preferably, the solvent adopts water and ethanol, and the mass ratio of the water to the ethanol is preferably 1:1.
in the step (2), preferably, the ultraviolet light has a wavelength of 10nm to 400nm; the power is 30W-200W.
In the step (2), the ultraviolet light irradiation time is preferably 5 minutes to 200 minutes, more preferably 10 minutes to 180 minutes, for example, 30 minutes, 60 minutes, 90 minutes, 150 minutes, 180 minutes, and most preferably 30 minutes to 90 minutes. From 5 minutes to 200 minutes, preferably from 10 minutes to 180 minutes, more preferably from 30 minutes to 90 minutes
The invention irradiates the suspension solution of the molybdenum oxide nano-sheet with ultraviolet light, increases the surface defect of the material, and can effectively improve the sensitivity of the molybdenum oxide nano-sheet to hydrogen sulfide. The treated molybdenum oxide nano-sheet maintains the selectivity and the moisture resistance to the hydrogen sulfide gas, and the resistance response to the hydrogen sulfide gas is improved compared with the resistance response before the treatment, so that the molybdenum oxide nano-sheet can be used for a resistance type hydrogen sulfide gas sensor. Namely, a resistance type hydrogen sulfide gas sensor comprises interdigital electrodes, wherein molybdenum oxide powder obtained after being treated by the method is dispersed in deionized water or ethanol to obtain slurry; the slurry is coated on the interdigital electrode and dried to form a film. The resistance type hydrogen sulfide gas sensor has the following beneficial effects:
(1) The detection sensitivity to hydrogen sulfide can be greatly improved, the lowest detection limit can reach 50ppb (ppb=1/1000 ppm), and the selectivity and the moisture resistance are higher.
(2) The operating temperature of the resistive hydrogen sulfide gas sensor is preferably 150 ℃ to 350 ℃, and more preferably 200 ℃ to 300 ℃, such as 200 ℃, 250 ℃, 300 ℃.
(3) The resistance response and the resistance recovery performance can be considered by adjusting the ultraviolet irradiation time and the working temperature of the sensor, and the method has good application prospect. For example, when the working temperature of the resistance type hydrogen sulfide gas sensor coated by the molybdenum oxide nano sheet obtained when the ultraviolet irradiation time is 30-60 minutes is 200-250 ℃, the resistance response to the hydrogen sulfide gas is excellent when the hydrogen sulfide gas is introduced, and meanwhile, the resistance can be restored to the initial value after the hydrogen sulfide gas is stopped to be introduced, namely, the resistance recovery capability is good. The resistance type hydrogen sulfide gas sensor is obtained by coating the molybdenum oxide nano sheet obtained by ultraviolet irradiation for 90-120 minutes, has excellent resistance response to the hydrogen sulfide gas when the hydrogen sulfide gas is introduced at the working temperature of 250-280 ℃, and has good resistance recovery capability when the resistance can be recovered to an initial value after the hydrogen sulfide gas is stopped being introduced.
(4) The resistance type hydrogen sulfide gas sensor is obtained by coating molybdenum oxide nano-sheets obtained by ultraviolet irradiation for 30 minutes, and has resistance response to 50ppb of hydrogen sulfide gas of more than 1, resistance response to 1ppm of hydrogen sulfide gas of more than 2.5, resistance response to 100ppb of hydrogen sulfide gas of more than 1.2 and resistance response to 10ppm of hydrogen sulfide gas of more than 350 when the working temperature is 200 ℃.
In the present invention, the resistance response (i.e., the multiple of resistance change) of the sensor is defined as: ra/Rg, wherein Ra is the resistance of the two ends of the interdigital electrode when the sensor is in a certain air atmosphere; rg is the resistance at two ends of the interdigital electrode when hydrogen sulfide gas with a certain concentration is introduced into the sensor under the condition of the same conditions.
Drawings
FIG. 1 is a photograph of each suspension after ultraviolet light irradiation in example 1.
Fig. 2 is a TEM image of each molybdenum oxide nanomaterial produced in example 1.
Fig. 3 is an XRD pattern of each molybdenum oxide nanomaterial produced in example 1.
Fig. 4 is XPS characterization results of each molybdenum oxide nanomaterial prepared in example 1.
FIG. 5 is a graph showing the resistive response of the sensor of example 1 to various gases at 150-350℃for 30 min.
FIG. 6 is the results of the moisture resistance test of the sensor of example 1 for 30 min.
FIG. 7 is a graph showing the resistance response of the sensor of example 1 when hydrogen sulfide gas was supplied at 0.5ppm to 30ppm for 0min.
FIG. 8 is the resistance response of the sensor of example 1 at 0.5ppm to 10ppm hydrogen sulfide gas feed-through for 30 min.
FIG. 9 is a graph showing the resistance response of the sensor of example 1 when hydrogen sulfide gas was supplied at 0.05ppm to 0.2ppm for 30 minutes.
FIG. 10 is a graph of the resistance response of the sensor of example 1 after heating to 150℃to 350℃and passing 10ppm hydrogen sulfide gas for 20 minutes.
FIG. 11 is a graph showing the resistance response of the sensor of example 1, which shows that the hydrogen sulfide gas was stopped after 10ppm of hydrogen sulfide gas was introduced at 200℃for 20 minutes.
Detailed Description
The following are specific examples of the present invention, and the technical solutions of the present invention are further described, but the present invention is not limited to these examples.
Example 1:
(1) Putting 100mg of molybdenum oxide nano-sheets into 100ml of solvent mixed by water and ethanol according to the volume ratio of 1:1, and stirring to form suspension;
(2) Repeating the step (1) for 6 times to obtain 6 parts of suspension, and placing each part of suspension under a 40w ultraviolet lamp for ultraviolet radiation, wherein the ultraviolet wavelength is 365nm, and the radiation time is 0min (i.e. no ultraviolet radiation is performed), 5min, 10min, 30min, 90min and 180min respectively;
a photograph of each suspension after UV irradiation is shown in FIG. 1, which shows that the molybdenum oxide suspension darkens from a pale blue to a dark blue.
(3) And (3) centrifugally drying each suspension after radiation to obtain molybdenum oxide powder.
The TEM images of the molybdenum oxide nano materials prepared above are shown in fig. 2, which shows that the ultraviolet irradiation has no influence on the morphology of the molybdenum oxide.
The XRD patterns of the respective molybdenum oxide nano-materials prepared above are shown in fig. 3, showing that the samples irradiated with ultraviolet light for 5 minutes, 10 minutes, 30 minutes, 90 minutes, 180 minutes are still molybdenum oxide, compared with the samples irradiated with ultraviolet light for 0 minutes, i.e., the ultraviolet light irradiation has no influence on the material phase.
The XPS characterization result of each molybdenum oxide nanomaterial prepared above is shown in fig. 4.
Wherein, the characterization of molybdenum and oxygen elements in the molybdenum oxide nano material prepared by irradiating for 5 minutes by ultraviolet light is shown in a graph (a) and a graph (b) in fig. 4;
the characterization of molybdenum and oxygen elements in the molybdenum oxide nano material prepared by ultraviolet irradiation for 10 minutes is shown in a graph (c) and a graph (d) in fig. 4;
the characterization of molybdenum and oxygen elements in the molybdenum oxide nano material prepared by ultraviolet irradiation for 30 minutes is shown in a graph (e) and a graph (f) in fig. 4;
the characterization of molybdenum and oxygen elements in the molybdenum oxide nano material prepared by irradiating with ultraviolet light for 90 minutes is shown in a graph (g) and a graph (h) in fig. 4;
the characterization of molybdenum and oxygen elements in the molybdenum oxide nano material prepared by irradiating the molybdenum oxide nano material for 180 minutes with ultraviolet light is shown in a graph (i) and a graph (j) in fig. 4.
As can be seen from fig. 4, as the ultraviolet irradiation time increases, 5 valent Mo (Mo 5+ ) And oxygen (O) is adsorbed by the defect ads ) An increase indicates an increase in surface defects of the material.
Mixing the molybdenum oxide powder prepared in the above manner into deionized water, and performing ultrasonic treatment for 30 minutes to obtain various slurries, wherein each slurry is respectively marked as slurry-0 min (namely, slurry prepared from molybdenum oxide nano material prepared by ultraviolet irradiation for 0min and the marks of other slurries are pushed in the same manner) according to the ultraviolet irradiation time, and slurry-5 min, slurry-10 min, slurry-30 min, slurry-90 min and slurry-180 min; each slurry is coated on a Jin Cha finger electrode of a resistance type hydrogen sulfide gas sensor, and the electrode is placed in a constant-temperature drying box at 100 ℃ for drying for more than 2 hours to form a film with good adhesion, and the sensor is respectively marked as a sensor-0 min (namely, the sensor obtained by coating the slurry-0 min, marks of other sensors and the like) according to the used slurry, a sensor-5 min, a sensor-10 min, a sensor-30 min, a sensor-90 min and a sensor-180 min.
Example 2:
each sensor prepared in example 1 was tested for resistance response to different gases in the range of 150-350 ℃. FIG. 5 is a graph of the results of a sensor-30 min test showing the selective sensitivity of the sensor to hydrogen sulfide gas compared to other gases.
Each sensor prepared in example 1 was tested for resistance change to hydrogen sulfide gas at different humidities. The graph of the resistance change of the sensor-30 min under the dry atmosphere with humidity of 0.57%, 1.28% and 2.12% is shown in fig. 6, and the humidity represents the volume percentage of the moisture in the atmosphere, which shows that the sensor has the moisture resistance. The test results of the remaining sensors are similar to those shown in fig. 5, i.e., each sensor has moisture resistance.
Example 3:
the hydrogen sulfide gas was tested by heating each sensor prepared in example 1 to 200 c as follows:
(1) Continuously introducing hydrogen sulfide gas with a certain concentration into the sensor for 20 minutes, and stopping introducing the hydrogen sulfide gas to recover the resistance of the sensor, wherein the time for stopping introducing the hydrogen sulfide gas is 20 minutes;
(2) The step (1) is repeated for a plurality of times, except that the hydrogen sulfide gas introduced each time is changed.
The results of the resistance response of the sensor when hydrogen sulfide gas was supplied at 0.5ppm to 30ppm for 0min are shown in FIG. 7, which shows that the sensor response was only 1.1 when the hydrogen sulfide gas concentration was 500 ppb.
The results of the resistance response of the sensor when hydrogen sulfide gas was supplied at 0.5ppm to 10ppm for 30min are shown in FIG. 8, and the sensor showed a response of 355.83 at 2pm, a response of 2.86 at 1ppm, and a response of 1.54 at 500ppb, when the concentration of hydrogen sulfide gas was 10 ppm.
The results of the resistance response when hydrogen sulfide gas was supplied at 0.05ppm to 0.2ppm to the sensor-30 min are shown in FIG. 9, which shows that the sensor response was 1.42 at a hydrogen sulfide gas concentration of 200ppb, 1.26 at 100ppb, and 1.07 at 50 ppb.
As can be seen from fig. 7 and 8, the resistance of the sensor-30 min at 200 ℃ can be restored to the initial state after stopping the hydrogen sulfide gas.
Example 4:
each sensor prepared in example 1 was heated to 150 ℃ to 350 ℃, 10ppm hydrogen sulfide gas was continuously introduced into the sensor for 20 minutes, then the hydrogen sulfide gas introduction was stopped, the resistance response of each sensor when hydrogen sulfide gas was introduced was observed, and the resistance recovery of each sensor after the hydrogen sulfide gas introduction was stopped was observed. The results are as follows.
The resistance response of each sensor when hydrogen sulfide gas was introduced is shown in FIG. 10, and the resistance change of the sensor-30 min at 150℃is shown in FIG. 11.
(1) As can be seen from FIG. 10, the resistance response of the sensor-30 min, the sensor-90 min, and the sensor-180 min is higher at 150-350 ℃ compared with the sensor-5 min and the sensor-10 min;
(2) As can be seen from fig. 10, for sensor-30 min, sensor-90 min, sensor-180 min, the lower the operating temperature, the greater the resistance response in the range of 150-350 ℃;
(3) As can be seen from FIG. 11, the sensor-30 min failed to recover the resistance to the initial state after stopping the hydrogen sulfide gas feed at 150 ℃. The test results of the sensor-30 min, the sensor-90 min and the sensor-180 min are similar to those of FIG. 11, and the resistance cannot be restored to the initial state after the hydrogen sulfide gas is stopped being introduced at 150 ℃;
(4) Through testing, the resistance of the sensor can be restored to the initial state after the hydrogen sulfide gas is stopped being introduced at 200 ℃ for-30 min; the resistance can not be restored to the initial state after the sensor-90 min and the sensor-180 min stop the hydrogen sulfide gas at 200 ℃;
the resistance can be restored to the initial state after the sensor-30 min and the sensor-90 min stop the hydrogen sulfide gas from being introduced at 250 ℃;
the resistance can be restored to the initial state after the hydrogen sulfide gas is stopped to be introduced at 300 ℃ for the sensor-30 min, the sensor-90 min and the sensor-180 min.
While the foregoing embodiments have been described in detail in connection with the embodiments of the invention, it should be understood that the foregoing embodiments are merely illustrative of the invention and are not intended to limit the invention, and any modifications, additions, substitutions and the like made within the principles of the invention are intended to be included within the scope of the invention.
Claims (12)
1. A method for improving sensitivity of molybdenum oxide nano-sheets to hydrogen sulfide is characterized by comprising the following steps: the molecular formula of the molybdenum oxide nano-sheet is MoO 3 The method comprises the following steps:
(1) Mixing molybdenum oxide nano-sheets with a solvent to form a suspension, wherein the solvent comprises one or two of water and ethanol;
(2) Carrying out ultraviolet radiation on the suspension, wherein the ultraviolet power is 30-200W, and the ultraviolet radiation time is 30-180 minutes;
(3) Drying the irradiated suspension to evaporate the solvent to obtain molybdenum oxide powder;
applying the molybdenum oxide powder to a resistive hydrogen sulfide gas sensor; the resistive hydrogen sulfide gas sensor comprises interdigital electrodes;
dispersing the molybdenum oxide powder in deionized water or ethanol to obtain slurry; coating the slurry on the interdigital electrode, and drying to form a film;
the lowest detection limit of the resistance type hydrogen sulfide gas sensor for hydrogen sulfide reaches 50 ppb.
2. The method as claimed in claim 1, wherein: the solvent adopts water and ethanol, and the mass ratio of the water to the ethanol is 1:1.
3. the method as claimed in claim 1, wherein: in the step (2), the ultraviolet light wavelength is 10nm-400nm.
4. The method as claimed in claim 1, wherein: in the step (2), the ultraviolet light irradiation time is 30 minutes to 90 minutes.
5. The method as claimed in claim 1, wherein: the working temperature of the resistance type hydrogen sulfide gas sensor is 150-350 ℃.
6. The method as claimed in claim 1, wherein: the working temperature of the resistance type hydrogen sulfide gas sensor is 200-300 ℃.
7. The method as claimed in claim 1, wherein: the ultraviolet irradiation time is 30 minutes to 60 minutes; the working temperature of the resistance type hydrogen sulfide gas sensor is 200-250 ℃.
8. The method as claimed in claim 1, wherein: the ultraviolet radiation time is 90-120 minutes, and the working temperature of the resistance type hydrogen sulfide gas sensor is 250-280 ℃.
9. The method as claimed in claim 1, wherein: the ultraviolet irradiation time is 30 minutes, and the resistance response to 50ppb of hydrogen sulfide gas is more than 1 when the operating temperature of the resistance type hydrogen sulfide gas sensor is 200 ℃.
10. The method as claimed in claim 9, wherein: the resistive response to 100ppb hydrogen sulfide gas is greater than 1.2.
11. The method as claimed in claim 9, wherein: the resistance response to 1ppm hydrogen sulfide gas is greater than 2.5.
12. The method as claimed in claim 9, wherein: the resistive response to 10ppm hydrogen sulfide gas is greater than 350.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101417817A (en) * | 2008-11-21 | 2009-04-29 | 中国地质大学（武汉） | Method for synthesizing photochromic nano MoO3 powder by hydrothermal method |
| CN101531401A (en) * | 2009-04-14 | 2009-09-16 | 中国地质大学（武汉） | Preparation method of MoO3 nanorod powder with sensitive photochromic property |
| KR101734733B1 (en) * | 2015-12-30 | 2017-05-11 | 현대자동차주식회사 | Color changeable hydrogen sensor based on molybdenum oxide and method of manufacturing the same |
| CN110879238A (en) * | 2019-10-25 | 2020-03-13 | 东北大学 | Molybdenum trioxide nano-structure sensitive material, corresponding ammonia gas sensor and preparation method |
| CN110967331A (en) * | 2019-12-06 | 2020-04-07 | 华东理工大学 | Oxidation-reduction-resistant amorphous MoO for SERS substrate3-xPreparation method and application of nanosheet |
| CN112730531A (en) * | 2020-12-24 | 2021-04-30 | 宁波大学 | Preparation method of hydrogen sulfide gas sensor based on molybdenum trioxide nanosheets |
| CN112852403A (en) * | 2021-01-05 | 2021-05-28 | 深圳技术大学 | Ultraviolet photochromic nano system and preparation method and application thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2006341550A1 (en) * | 2005-12-12 | 2007-10-18 | Nextech Materials, Ltd. | Ceramic H2S sensor |
-
2022
- 2022-03-15 CN CN202210251087.4A patent/CN114620767B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101417817A (en) * | 2008-11-21 | 2009-04-29 | 中国地质大学（武汉） | Method for synthesizing photochromic nano MoO3 powder by hydrothermal method |
| CN101531401A (en) * | 2009-04-14 | 2009-09-16 | 中国地质大学（武汉） | Preparation method of MoO3 nanorod powder with sensitive photochromic property |
| KR101734733B1 (en) * | 2015-12-30 | 2017-05-11 | 현대자동차주식회사 | Color changeable hydrogen sensor based on molybdenum oxide and method of manufacturing the same |
| CN110879238A (en) * | 2019-10-25 | 2020-03-13 | 东北大学 | Molybdenum trioxide nano-structure sensitive material, corresponding ammonia gas sensor and preparation method |
| CN110967331A (en) * | 2019-12-06 | 2020-04-07 | 华东理工大学 | Oxidation-reduction-resistant amorphous MoO for SERS substrate3-xPreparation method and application of nanosheet |
| CN112730531A (en) * | 2020-12-24 | 2021-04-30 | 宁波大学 | Preparation method of hydrogen sulfide gas sensor based on molybdenum trioxide nanosheets |
| CN112852403A (en) * | 2021-01-05 | 2021-05-28 | 深圳技术大学 | Ultraviolet photochromic nano system and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 氧化钼基纳米材料的制备及气敏性能研究;沈士凯;中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》(第4期);第19页、第21页和第54页 * |
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