CN114609197A - Gas sensitive material, preparation method and application thereof in NH3Application in gas sensor - Google Patents
Gas sensitive material, preparation method and application thereof in NH3Application in gas sensor Download PDFInfo
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- CN114609197A CN114609197A CN202210299257.6A CN202210299257A CN114609197A CN 114609197 A CN114609197 A CN 114609197A CN 202210299257 A CN202210299257 A CN 202210299257A CN 114609197 A CN114609197 A CN 114609197A
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- 239000000463 material Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 150
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 106
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 97
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 14
- 230000035945 sensitivity Effects 0.000 claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 11
- 239000000919 ceramic Substances 0.000 claims abstract description 9
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000010931 gold Substances 0.000 claims abstract description 9
- 229910052737 gold Inorganic materials 0.000 claims abstract description 9
- 238000011065 in-situ storage Methods 0.000 claims abstract description 7
- 239000011248 coating agent Substances 0.000 claims abstract description 5
- 238000000576 coating method Methods 0.000 claims abstract description 5
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 claims description 56
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- 229930192474 thiophene Natural products 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 25
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 24
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 20
- 239000006185 dispersion Substances 0.000 claims description 19
- 239000007788 liquid Substances 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 239000000178 monomer Substances 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 16
- 239000011258 core-shell material Substances 0.000 claims description 15
- 238000005303 weighing Methods 0.000 claims description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 11
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 10
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 10
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 5
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 5
- 229910000069 nitrogen hydride Inorganic materials 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 150000004685 tetrahydrates Chemical class 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 5
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000003466 welding Methods 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 6
- 238000011084 recovery Methods 0.000 abstract description 5
- 230000004044 response Effects 0.000 abstract description 5
- 239000002131 composite material Substances 0.000 abstract description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 239000002243 precursor Substances 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 54
- 229910021529 ammonia Inorganic materials 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 229920000123 polythiophene Polymers 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004043 responsiveness Effects 0.000 description 2
- 239000011540 sensing material Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- -1 5-substituted thiophene ring Chemical group 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
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- 238000013329 compounding Methods 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
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- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- G01N27/126—Composition of the body, e.g. the composition of its sensitive layer comprising organic polymers
Abstract
The invention provides a method based on MoO3@MoS2A/PTH composite material, a preparation method and application in an ammonia gas sensor relate to the field of gas detection, wherein MoO3@MoS2Account for MoO3@MoS220% of PTH mass fraction; the working temperature is room temperature, and the sensitivity to 50ppm ammonia gas reaches 1.4; the preparation method comprises the following steps: firstly, flower-shaped MoO is prepared by a hydrothermal method3In MoO3Preparation of MoO for precursors3@MoS2Then preparing MoO by in-situ polymerization3@MoS2A PTH gas sensitive material; adding MoO3@MoS2Coating PTH material on gold electrode coated Al2O3The surface of the ceramic tube is made into a gas-sensitive element. MoO prepared by in-situ polymerization method3@MoS2The PTH gas-sensitive material has high sensitivity to ammonia gas, and fast response time and recovery time.
Description
Technical Field
The invention relates to the technical field of functional nano material preparation and the technical field of gas sensor detection, in particular to a gas sensitive material, a preparation method and application thereof in a gas sensor.
Background
In recent years, with the rapid development of modern industry, environmental and ecological problems are more and more emphasized by people, environmental protection and monitoring of harmful substances become urgent, air pollution is closely related to human health, and detection of harmful gases is more and more needed. Ammonia is a common gas in daily life, is not only a raw material of many chemical products, but also an exhaust gas of many chemical products, and when the index concentration of ammonia exceeds a certain range, the ammonia can cause damage to our bodies, so that the ammonia concentration needs to be monitored to ensure the product quality and the environmental safety.
There are many kinds of chemical resistance sensors on the world, and the sensors using metal semiconductors as sensitive materials are many, and the sensitivity of semiconductor sensors is high, but the use temperature is high, and the gas selectivity is poor, so that a novel resistance sensor is urgently needed, and the applicability and the selectivity of the sensor are improved. The polythiophene in the conductive polymer is considered to be a promising sensing material because of the advantages of easy polymerization, high conductivity, good thermal stability, environmental stability and the like, and the synergistic effect or complementary effect between the polythiophene and the inorganic component has important significance for improving the gas-sensitive performance of components.
In recent years, new two-dimensional materials have rapidly developed, among which MoS2Has the characteristics of good conductivity, strong adsorption force, high reaction activity, good flexibility and the like, and has natural band gap. MoS2Is a strict two-dimensional material, has large specific surface area, has unsaturated bonds at the edge and the like, and provides active sites for gas molecule adsorption reaction. These characteristics are such that MoS2The material becomes a hot spot for researching the gas-sensitive sensing material. MoS2Is not sensitive to certain gasesTherefore, the gas-sensitive performance of the gas sensor is improved by adopting a doping and compounding means, and a new thought is provided for the development of the gas-sensitive device with the superior performances of low detection limit, high responsiveness, short response/recovery time, low production cost and the like.
MoO3The wide-band transition metal oxide semiconductor material has a special layer structure, good oxidation-reduction catalytic activity and stable physical and chemical properties, can better control the morphology structure by controlling reaction conditions, and improves the gas-sensitive performance of the material by doping and heterojunction construction.
The CN105510403A invention adopts a chemical or physical etching method to form a quasi-periodic structure on the surface of a monocrystalline silicon piece, and an electrode is formed by thermal evaporation coating to detect ammonia gas, but the process has high requirements on equipment, high operation requirements and high production cost, and is not beneficial to large-scale application. CN102978578A adopts the sputtering method to prepare the copper oxide doped tin dioxide matrix ammonia gas sensor, the sensitivity of the sensor is high and the response recovery time is short, but the working temperature is high and the volume is large. CN104502415A invented an ammonia gas sensor based on a precious metal composite material, which has good gas-sensitive performance but high cost. CN110702752 invented a catalytic gas sensor, but its recovery time was long. CN102103103A discloses a sensor for detecting ammonia gas and a method for making the same, which is made of an organic thin film transistor for detecting ammonia gas, but the transistor sensor has the disadvantages of complex processing technology, long manufacturing period, harsh manufacturing conditions, and unfriendly environment of chemical reagents used in the manufacturing process.
In view of this, the invention provides a gas sensor and an application thereof in ammonia gas detection, which are used for solving the defect that the gas sensor can work only when being heated or under an ultraviolet lamp in the prior art.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a MoO3@MoS2A PTH gas-sensitive material, a preparation method and application thereof in a gas-sensitive sensor.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a gas-sensitive material is MoO3@MoS2PTH by MoO3As nucleus, with MoS2MoO forming a core-shell structure for the shell3@MoS2Then polymerized with thiophene monomer, wherein MoO3And MoS2Core-shell structure MoO3@MoS2The weight percentage of the material is 10-30%.
As a preferable mode, firstly, the flower-shaped nano molybdenum trioxide is prepared by a hydrothermal method, and then MoO is prepared3And MoS2Core-shell structure, preparation of MoO by in-situ polymerization3@MoS2/PTH。
Preferably, the gas-sensitive material is of a sheet stacking structure, and the MoO3@MoS2The working temperature of the/PTH gas-sensitive material is room temperature, and the sensitivity of the PTH gas-sensitive material to 50ppm ammonia gas reaches 1.4.
The invention also provides a preparation method of the gas sensitive material, which comprises the following steps:
s1: preparing flower-shaped molybdenum trioxide: mixing a mixture of 1: heptamolybdic acid tetrahydrate of 10 to 3:10 (NH)4)6Mo7O24·4H2O and ammonium sulfate (NH)4)2SO4Dissolving the mixture in 50mL of deionized water, continuously adding 0.93mol of ammonia water and a proper amount of deionized water to a constant volume of 70mL, uniformly stirring the obtained solution, adding 1.817g of thioacetamide, uniformly stirring to obtain a clear solution, transferring the solution to a 100mL hydrothermal reaction kettle, and heating at 180-240 ℃ for 24 hours; naturally cooling to room temperature, collecting the obtained precipitate, washing with deionized water and ethanol for several times, and vacuum drying at 60 deg.C for 10 hr;
s2: preparation of MoO3@MoS2: 1mM of MoO was weighed3Ultrasonically dispersing the powder into 100mL of mixed solution of water and ethanol, wherein the volume ratio of the water to the ethanol in the mixed solution is 2:3, and homogenizing to obtain MoO3After dispersion, thiourea, MoO was added in different molar ratios3：H2NSNH2In a molar ratio of1: 1-1: 10, when thiourea is completely dissolved, transferring the whole mixed dispersion liquid into a hydrothermal kettle with the capacity of 100mL, wherein the filling ratio of the hydrothermal kettle is 70%, the hydrothermal temperature is 180-220 ℃, and the hydrothermal time is 18-24 h; after the reaction is finished, cooling to room temperature, respectively centrifugally washing with water and ethanol for a plurality of times, and drying to obtain MoO3@MoS2；
S3: preparing materials, weighing anhydrous ferric chloride, dissolving in chloroform, stirring for 1h to obtain dark green turbid liquid, weighing thiophene monomer and MoO3@MoS2Dissolving in chloroform, thiophene monomer and MoO3@MoS2The mass ratio of thiophene to molybdenum disulfide is 10: 1-10: 3, ultrasonic treatment is carried out for 1 hour to obtain a dispersion liquid of thiophene and molybdenum disulfide, the dispersion liquid is slowly dripped into turbid ferric chloride night, and stirring reaction is carried out at room temperature for 9 hours; after the reaction is finished, evaporating the solvent to dryness at room temperature, adding a proper amount of 1mol/L HCI, and stirring at room temperature for 12 hours; and washing the obtained product with HCl for multiple times, washing with deionized water, and drying at 60-80 ℃ for 6-8 hours.
Preferably, in S1, the solution is transferred to a hydrothermal reaction kettle and reacted at 180 ℃ for 24 h.
Preferably, in S2, MoO is weighed in a molar ratio of 1:33And H2NSNH2Added to the solution.
Preferably, in S3, weighing thiophene monomer and MoO with the mass ratio of 10:23@MoS2Dissolved in chloroform.
The invention also provides a gas sensitive material in NH3Use in a gas sensor, which is: adding MoO3@MoS2Al coated with PTH sensitive material and coated with gold electrode2O3The surface of the ceramic tube is made into a gas-sensitive sensing element.
Preferably, the NH is3The preparation method of the gas-sensitive sensing element comprises the following steps: get MoO3@MoS2Grinding PTH powder product for 10min, adding anhydrous ethanol, mixing, grinding to paste, and uniformly coating the paste on Al coated with gold electrode2O3Evaporating ethanol to dryness at room temperature on the surface of the ceramic tube, and welding a gold electrode on a ceramic base。
The invention has the beneficial effects that: the invention provides a gas sensor which can detect ammonia gas with different concentrations under the condition of normal-temperature visible light and has the advantages of good responsiveness, high sensitivity, quick response and recovery time and strong selectivity; and the preparation is simple, the production cost is low, and the method is suitable for ammonia detection in certain environments. The technical defect that the gas sensor can work only under high temperature or ultraviolet light in the prior art is overcome.
Drawings
FIG. 1 is a flower-like MoO of the present invention3SEM image of (d). (a) At low magnification, (b) at high magnification
FIG. 2 is an SEM image of a polythiophene according to the present invention. (a) At low magnification, (b) at high magnification
FIG. 3 is a MoO of the present invention3@MoS2SEM image of/PTH. (a) At low magnification, (b) at high magnification
FIG. 4 is a MoO of the present invention3@MoS2XPS plot of/PTH.
FIG. 5 shows PTH and MoO of the present invention3@MoS2、MoO3@MoS2FTIR plot of/PTH.
FIG. 6 shows MoO at room temperature according to the present invention3@MoS2the/PTH response curves for ammonia gas at different concentrations.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Example 1
This example provides a gas sensitive material, which is MoO3@MoS2PTH by MoO3As nucleus, with MoS2Forming a core-shell structure MoO for the shell3@MoS2Then with thiophene monomersIs polymerized to obtain MoO3And MoS2Core-shell structure MoO3@MoS2The weight percentage of the material is 10-30%.
The gas sensitive material is of a sheet stacking structure, and the MoO3@MoS2The working temperature of the/PTH gas-sensitive material is room temperature, and the sensitivity of the PTH gas-sensitive material to 50ppm ammonia gas reaches 1.4.
The embodiment also provides a preparation method of the gas-sensitive material, which comprises the steps of firstly preparing flower-shaped nano molybdenum trioxide by a hydrothermal method, and then preparing MoO3And MoS2Core-shell structure, preparation of MoO by in-situ polymerization3@MoS2/PTH。
The method specifically comprises the following steps:
s1: preparing flower-shaped molybdenum trioxide: mixing a mixture of 1:10 heptamolybdic acid tetrahydrate of (NH)4)6Mo7O24·4H2O and ammonium sulfate (NH)4)2SO4Dissolving the mixture in 50mL of deionized water, continuously adding 0.93mol of ammonia water and a proper amount of deionized water to a constant volume of 70mL, uniformly stirring the obtained solution, adding 1.817g of thioacetamide, uniformly stirring to obtain a clear solution, transferring the solution to a 100mL hydrothermal reaction kettle, and heating at 180 ℃ for 24 hours; naturally cooling to room temperature, collecting the obtained precipitate, washing with deionized water and ethanol for several times, and vacuum drying at 60 deg.C for 10 hr;
s2: preparation of MoO3@MoS2: 1mM of MoO was weighed3Ultrasonically dispersing the powder into 100mL of mixed solution of water and ethanol, wherein the volume ratio of the water to the ethanol in the mixed solution is 2:3, and homogenizing to obtain MoO3After dispersion, different molar ratios of thiourea, MoO were added3：H2NSNH2When thiourea is completely dissolved, transferring the whole mixed dispersion liquid into a hydrothermal kettle with the capacity of 100mL, wherein the filling ratio of the hydrothermal kettle is 70%, the hydrothermal temperature is 180 ℃, and the hydrothermal time is 24 h; after the reaction is finished, cooling to room temperature, respectively centrifugally washing with water and ethanol for a plurality of times, and drying to obtain MoO3@MoS2；
S3: preparing materials, weighing anhydrous ferric chloride, dissolving in chloroform, stirring for 1h to obtain dark green turbid liquid, weighing thiophene monomer and MoO3@MoS2Dissolving in chloroform, thiophene monomer and MoO3@MoS2The mass ratio of thiophene to molybdenum disulfide is 10:1, ultrasonic treatment is carried out for 1h to obtain a dispersion liquid of thiophene and molybdenum disulfide, the dispersion liquid is slowly dripped into turbid ferric chloride, and stirring reaction is carried out at room temperature for 9 h; after the reaction is finished, evaporating the solvent to dryness at room temperature, adding a proper amount of 1mol/L HCI, and stirring at room temperature for 12 hours; the resulting product was washed several times with HCl, then with deionized water and dried at 60 ℃ for 6 hours.
Example 2
This example provides a gas sensitive material, which is MoO3@MoS2PTH by MoO3As nucleus, with MoS2MoO forming a core-shell structure for the shell3@MoS2Then polymerized with thiophene monomer, wherein MoO3And MoS2Core-shell structure MoO3@MoS2The weight percentage of the material is 10-30%.
The gas sensitive material is of a sheet stacking structure, and the MoO3@MoS2The working temperature of the/PTH gas-sensitive material is room temperature, and the sensitivity of the PTH gas-sensitive material to 50ppm ammonia gas reaches 1.4.
The embodiment also provides a preparation method of the gas-sensitive material, which comprises the steps of firstly preparing flower-shaped nano molybdenum trioxide by a hydrothermal method, and then preparing MoO3And MoS2Core-shell structure, preparation of MoO by in-situ polymerization3@MoS2/PTH。
The method specifically comprises the following steps:
s1: preparing flower-shaped molybdenum trioxide: heptamolybdic acid tetrahydrate in a molar ratio of 3:10 (NH)4)6Mo7O24·4H2O and ammonium sulfate (NH)4)2SO4Dissolving in 50mL of deionized water, continuously adding 0.93mol of ammonia water and a proper amount of deionized water to constant volume of 70mL, uniformly stirring the obtained solution, adding 1.817g of thioacetamide, uniformly stirring to obtain a clear solution, and transferring the solution to 100mL of hydrothermal solutionHeating in a reaction kettle at 240 ℃ for 24 hours; naturally cooling to room temperature, collecting the obtained precipitate, washing with deionized water and ethanol for several times, and vacuum drying at 60 deg.C for 10 hr;
s2: preparation of MoO3@MoS2: 1mM of MoO was weighed3Ultrasonically dispersing the powder into 100mL of mixed solution of water and ethanol, wherein the volume ratio of the water to the ethanol in the mixed solution is 2:3, and homogenizing to obtain MoO3After dispersion, different molar ratios of thiourea, MoO were added3：H2NSNH2When thiourea is completely dissolved, transferring the whole mixed dispersion liquid into a hydrothermal kettle with the capacity of 100mL, wherein the filling ratio of the hydrothermal kettle is 70%, the hydrothermal temperature is 220 ℃, and the hydrothermal time is 18 h; after the reaction is finished, cooling to room temperature, respectively centrifugally washing with water and ethanol for a plurality of times, and drying to obtain MoO3@MoS2；
S3: preparing materials, weighing anhydrous ferric chloride, dissolving in chloroform, stirring for 1h to obtain dark green turbid liquid, weighing thiophene monomer and MoO3@MoS2Dissolving in chloroform, thiophene monomer and MoO3@MoS2The mass ratio of thiophene to molybdenum disulfide is 10:3, ultrasonic treatment is carried out for 1h to obtain a dispersion liquid of thiophene and molybdenum disulfide, the dispersion liquid is slowly dripped into turbid ferric chloride, and stirring reaction is carried out at room temperature for 9 h; after the reaction is finished, evaporating the solvent to dryness at room temperature, adding a proper amount of 1mol/L HCI, and stirring at room temperature for 12 hours; and washing the obtained product with HCl for multiple times, washing with deionized water, and drying at 60-80 ℃ for 6-8 hours.
Example 3
This example provides a gas sensitive material, which is MoO3@MoS2PTH by MoO3As nucleus, with MoS2Forming a core-shell structure MoO for the shell3@MoS2Then polymerized with thiophene monomer, wherein MoO3And MoS2Core-shell structure MoO3@MoS2The weight percentage of the material is 10-30%.
The gas sensitive material is of a sheet stacking structure, and the MoO3@MoS2The working temperature of the PTH gas-sensitive material is room temperatureThe sensitivity to 50ppm of ammonia gas reached 1.4.
The embodiment also provides a preparation method of the gas-sensitive material, which comprises the steps of firstly preparing flower-shaped nano molybdenum trioxide by a hydrothermal method, and then preparing MoO3And MoS2Core-shell structure, preparation of MoO by in-situ polymerization3@MoS2/PTH。
The method specifically comprises the following steps:
s1: preparing flower-shaped molybdenum trioxide: mixing the components in a molar ratio of 2: 10 heptamolybdic acid tetrahydrate of (NH)4)6Mo7O24·4H2O and ammonium sulfate (NH)4)2SO4Dissolving the mixture in 50mL of deionized water, continuously adding 0.93mol of ammonia water and a proper amount of deionized water to a constant volume of 70mL, uniformly stirring the obtained solution, adding 1.817g of thioacetamide, uniformly stirring to obtain a clear solution, transferring the solution to a 100mL hydrothermal reaction kettle, and heating at 200 ℃ for 24 hours; naturally cooling to room temperature, collecting the obtained precipitate, washing with deionized water and ethanol for several times, and finally vacuum drying at 60 deg.C for 10 hr;
s2: preparation of MoO3@MoS2: 1mM of MoO was weighed3Ultrasonically dispersing the powder into 100mL of mixed solution of water and ethanol, wherein the volume ratio of the water to the ethanol in the mixed solution is 2:3, and homogenizing to obtain MoO3After dispersion, different molar ratios of thiourea, MoO were added3：H2NSNH2When thiourea is completely dissolved, transferring the whole mixed dispersion liquid into a hydrothermal kettle with the capacity of 100mL, wherein the filling ratio of the hydrothermal kettle is 70%, the hydrothermal temperature is 200 ℃, and the hydrothermal time is 20 h; after the reaction is finished, cooling to room temperature, respectively centrifugally washing with water and ethanol for a plurality of times, and drying to obtain MoO3@MoS2；
S3: preparing materials, weighing anhydrous ferric chloride, dissolving in chloroform, stirring for 1h to obtain dark green turbid liquid, weighing thiophene monomer and MoO3@MoS2Dissolving in chloroform, thiophene monomer and MoO3@MoS2The mass ratio of (A) to (B) is 10:2, and the ultrasonic treatment is carried out for 1hAdding the dispersion liquid of thiophene and molybdenum disulfide slowly dropwise into turbid ferric chloride solution, and stirring and reacting for 9 hours at room temperature; after the reaction is finished, evaporating the solvent to dryness at room temperature, adding a proper amount of 1mol/L HCI, and stirring at room temperature for 12 hours; the resulting product was washed with HCl several times, then with deionized water and dried at 70 ℃ for 7 hours.
Performance testing
MoO for 3 examples3@MoS2Characterization of the/PTH gas sensitive material:
MoO prepared by using scanning electron microscope, Fourier infrared spectrometer and X-ray photoelectron spectrometer3@MoS2the/PTH gas sensitive material was physically or chemically characterized, yielding fig. 1, fig. 2, fig. 3, fig. 4, fig. 5, respectively:
FIG. 1 is MoO3Scanning electron micrograph of (1), from which the resulting MoO can be seen3Is in a flower-shaped structure;
FIG. 2 is a scanning electron microscope image of polythiophene, wherein synthetic rod-shaped polythiophene can be seen from the image, and is connected into a net structure;
FIG. 3 is MoO3@MoS2Scanning electron microscope image of/PTH, from which it can be seen that PTH succeeds in MoO3@MoS2The polymerization is successfully carried out;
FIG. 4 shows MoO3@MoS2X-ray photoelectron spectrum of/PTH: the composite material can be seen from the figure consisting of C, O, S, Mo and four elements, and four peaks shown in 164.41eV, 229.08eV, 285.07eV and 532.33eV are respectively assigned to the binding energies of S2p, Mo3d, C1S and O1S.
FIG. 5 shows PTH and MoO3@MoS2、MoO3@MoS2FT-IR picture of/PTH, MoO3@MoS2the/PTH nanocomposite showed peaks similar to PTH. 785.03cm-1The position corresponds to the out-of-plane C-H stretching vibration of the 2, 5-substituted thiophene ring generated by the polymerization of the thiophene monomer. 670.5cm-1The peak value of (A) is C-S bond bending vibration, 462.92cm-1The peak band at (A) can be attributed to the ring deformation mode of the C-S-C bond, demonstrating that thiophene is in MoO3@MoS2The polymerization was successful.
Example 4 preparationMoO3@MoS2PTH ammonia gas sensor
Get MoO3@MoS2Grinding PTH powder product for 10min, adding anhydrous ethanol, mixing, grinding to paste, and uniformly coating the paste on Al coated with gold electrode2O3Evaporating ethanol to dryness at room temperature on the surface of the ceramic tube, and welding a gold electrode on a ceramic base to obtain NH3A gas sensor.
For MoO of example 43@MoS2Sensitivity of/PTH ammonia gas sensor is tested
The sensitivity of the gas-sensitive material is measured by adopting a static gas distribution method: MoO prepared at room temperature3@MoS2The PTH sensor is tested by adding ammonia gas with different concentrations and using S ═ R/R0The sensitivity for different concentrations is calculated by the formula, where R is the resistance of the sensor after exposure to ammonia gas and R is the resistance of the sensor after exposure to ammonia gas0Is the initial resistance value of the sensor in air to obtain MoO3@MoS2The sensitivity of the/PTH gas sensitive material to 50ppm, 100ppm, 200ppm, 300ppm, 500ppm, 800ppm is shown in FIG. 6.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Those skilled in the art can modify or change the above-described embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (9)
1. A gas-sensitive material characterized by: the material is MoO3@MoS2PTH by MoO3As nucleus, with MoS2Forming a core-shell structure MoO for the shell3@MoS2Then polymerized with thiophene monomer, wherein MoO3And MoS2Core-shell structure MoO3@MoS2The weight percentage of the material is 10-30%.
2. The gas-sensitive material of claim 1, wherein: firstly, preparing flower-shaped nano molybdenum trioxide by a hydrothermal method, and then preparing MoO3And MoS2Core-shell structure, preparation of MoO by in-situ polymerization3@MoS2/PTH。
3. The gas-sensitive material of claim 1, wherein: the gas sensitive material is of a sheet stacking structure, and the MoO3@MoS2The working temperature of the/PTH gas-sensitive material is room temperature, and the sensitivity of the PTH gas-sensitive material to 50ppm ammonia gas reaches 1.4.
4. A method for producing the gas-sensitive material according to any one of claims 1 to 3, characterized in that: the method specifically comprises the following steps:
s1: preparing flower-shaped molybdenum trioxide: mixing a mixture of 1: heptamolybdic acid tetrahydrate of 10 to 3:10 (NH)4)6Mo7O24·4H2O and ammonium sulfate (NH)4)2SO4Dissolving the mixture in 50mL of deionized water, continuously adding 0.93mol of ammonia water and a proper amount of deionized water to a constant volume of 70mL, uniformly stirring the obtained solution, adding 1.817g of thioacetamide, uniformly stirring to obtain a clear solution, transferring the solution to a 100mL hydrothermal reaction kettle, and heating at 180-240 ℃ for 24 hours; naturally cooling to room temperature, collecting the obtained precipitate, washing with deionized water and ethanol for several times, and vacuum drying at 60 deg.C for 10 hr;
s2: preparation of MoO3@MoS2: 1mM MoO was weighed3Ultrasonically dispersing the powder into 100mL of mixed solution of water and ethanol, wherein the volume ratio of the water to the ethanol in the mixed solution is 2:3, and homogenizing to obtain MoO3After dispersion, different molar ratios of thiourea, MoO were added3：H2NSNH2The molar ratio of the thiourea to the solvent is 1: 1-1: 10, when the thiourea is completely dissolved, transferring the whole mixed dispersion liquid into a hydrothermal kettle with the capacity of 100mL, wherein the filling ratio of the hydrothermal kettle is 70%, the hydrothermal temperature is 180-220 ℃, and the hydrothermal time is 18-24 h; after the reaction is finished, cooling to room temperature, and respectively using water and BCentrifugally washing with alcohol for several times, and drying to obtain MoO3@MoS2；
S3: preparing materials, weighing anhydrous ferric chloride, dissolving in chloroform, stirring for 1h to obtain dark green turbid liquid, weighing thiophene monomer and MoO3@MoS2Dissolving in chloroform, thiophene monomer and MoO3@MoS2The mass ratio of thiophene to molybdenum disulfide is 10: 1-10: 3, ultrasonic treatment is carried out for 1 hour to obtain a dispersion liquid of thiophene and molybdenum disulfide, the dispersion liquid is slowly dripped into turbid ferric chloride night, and stirring reaction is carried out at room temperature for 9 hours; after the reaction is finished, evaporating the solvent to dryness at room temperature, adding a proper amount of 1mol/L HCI, and stirring at room temperature for 12 hours; and washing the obtained product with HCl for multiple times, washing with deionized water, and drying at 60-80 ℃ for 6-8 hours.
5. The method for preparing a gas-sensitive material according to claim 4, wherein: in S1, the solution is transferred to a hydrothermal reaction kettle and reacted for 24 hours at 180 ℃.
6. The method for preparing a gas-sensitive material according to claim 4, wherein: in S2, MoO with a molar ratio of 1:3 is weighed3And H2NSNH2Added to the solution.
7. The method of claim 4, wherein: in S3, weighing thiophene monomers and MoO in a mass ratio of 10:23@MoS2Dissolved in chloroform.
8. Gas sensitive material in NH3Use in a gas sensor, characterized in that: adding MoO3@MoS2Al coated with PTH sensitive material and coated with gold electrode2O3Making NH on the surface of the ceramic tube3A gas sensor element.
9. Gas sensitive material according to claim 8 in NH3Use in a gas sensor, characterized in that: the NH3The preparation method of the gas-sensitive sensing elementThe following were used: get MoO3@MoS2Grinding PTH powder for 10min, adding anhydrous ethanol, mixing, grinding to paste, and uniformly coating the paste on Al coated with gold electrode2O3And (3) evaporating the ethanol to dryness at room temperature on the surface of the ceramic tube, and welding the gold electrode on the ceramic base.
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