CN111007114A - Preparation method of gas-sensitive film based on photosynthesis mechanism and gas sensor - Google Patents
Preparation method of gas-sensitive film based on photosynthesis mechanism and gas sensor Download PDFInfo
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- CN111007114A CN111007114A CN201911169526.1A CN201911169526A CN111007114A CN 111007114 A CN111007114 A CN 111007114A CN 201911169526 A CN201911169526 A CN 201911169526A CN 111007114 A CN111007114 A CN 111007114A
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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
Abstract
The invention provides a preparation method of a gas-sensitive film based on a photosynthesis mechanism and a gas sensor, belonging to the technical field of gas sensing, wherein the method comprises the following steps: (1) stirring the PS I metal oxide precursor under the water bath condition to obtain a PS I metal oxide precursor solution; (2) mixing a metal nanoparticle precursor with a PS I metal oxide precursor solution, and stirring under a water bath condition to obtain a mixed solvent; (3) dispersing PS II metal oxide particles in a mixed solvent; (4) adding diethanolamine, stirring, and dropwise adding ammonia water to adjust the pH value of the solution to obtain stable and uniform sol; (5) standing and aging the prepared sol at room temperature; (6) and drying in a drying box, grinding into fine powder, and calcining in a muffle furnace to obtain the gas-sensitive membrane. The method can effectively promote the effective separation of photo-generated charges in the gas-sensitive detection process, and also solves the problem of insufficient oxidation-reduction capability of the traditional heterostructure, so that photo-excited charges are utilized most fully.
Description
Technical Field
The invention relates to the technical field of gas sensing, in particular to a preparation method of a gas-sensitive film based on a photosynthesis mechanism and a gas sensor.
Background
The correct identification and sensitive response to the trace components in the complex background are always hot points and difficulties in the research of the gas sensor, and on the basis of optimizing the existing detection technology, the exploration of a new gas-sensitive mechanism and the development of a reliable and feasible detection method have important significance. In order to accurately analyze and detect toxic and harmful gases in the environment, almost all analytical testing methods including chromatography (GC), Mass Spectrometry (MS), Capillary Electrophoresis (CE), chromatography-mass spectrometry (GC-MS), chromatography-detector combination, and the like have been tried. However, these instruments are bulky, complicated to operate, long in analysis time, expensive, require the presence of a professional, are difficult to perform on-line automatic monitoring, or have a need for rapid emergency response to an emergency. Therefore, the development of a highly sensitive, highly selective, portable, low-cost gas sensor is urgently needed.
Researchers at home and abroad have already developed sensors for detecting toxic and harmful gases in various environments, mainly comprising quartz crystal microbalances QCM, surface acoustic wave SAW and semiconductor resistance type gas sensors. However, although QCM and SAW sensors have high sensitivity to a gas to be detected, they have poor baseline stability and are sensitive to the external environment, especially factors such as airflow and temperature, and a weak signal to be detected may be covered by fluctuation of a substrate signal to a great extent and is difficult to acquire. The oxide semiconductor gas sensor has the characteristics of higher sensitivity to other gases as found in the detection test of toxic and harmful gases. However, gas-sensitive detection under heating is required to achieve optimal sensitivity, and power consumption is large and IC integration is inconvenient.
Thus, researchers have attempted to prepare photo-assisted semiconductor gas Sensors at room temperature, J.Saurazani, Astro Yanbalilo atomic energy research center, ①, see Sensors and promoters B: Chemical, 17, 1994, 211- "214, first discovered SnO under ultraviolet light in 19942The gas sensor has good response to acetone, and researchers in various countries put a lot of work on ZnO and TiO2、WO3Isosemiconductor gas sensitive materialAnd (5) feeding. To further improve the detection sensitivity, Deng, Sensors and activators B: synthesis of porous CuO-SnO by impregnation method used in Chemical 297, 2019, 1268162A heterogeneous structure is constructed by compounding semiconductors, a large number of electron-hole pairs are generated in a grain boundary depletion layer under the assistance of ultraviolet light, the height of a grain boundary potential barrier is reduced, and the gas detection limit is improved. The conventional heterostructure can promote the effective separation of photo-generated charges as shown in fig. 1, however, after the transfer of the photo-generated charges, photo-generated electrons are positioned on the conduction band of the semiconductor II with the corrected conduction band potential, and the reduction capability is weakened; accordingly, the photogenerated holes migrate to the valence band of the more negative potential semiconductor I and the oxidation capability is diminished. As such, practical application of the heterogeneous composite material is necessarily limited. The problems that the photo-generated electron-hole pairs of the semiconductor material are easy to recombine and the conventional heterostructure has insufficient oxidation-reduction capability are not always solved positively.
Disclosure of Invention
Aiming at the defects that the photo-generated electron-hole pairs of the single semiconductor material are easy to compound and the conventional heterostructure is insufficient in oxidation-reduction capability, so that photo-excited charges cannot be fully utilized, the invention aims to provide a preparation method of a gas-sensitive film based on a photosynthesis mechanism and a gas sensor.
A preparation method of a gas-sensitive film based on a photosynthesis mechanism comprises the following steps:
(1) stirring the PS I metal oxide precursor under the water bath condition to obtain a PS I metal oxide precursor solution;
(2) mixing a metal nanoparticle precursor with the PS I metal oxide precursor solution obtained in the step (1), and stirring under a water bath condition to obtain a mixed solvent;
(3) dispersing PS II metal oxide particles in the mixed solvent obtained in the step (2), stirring under a water bath condition, and then carrying out ultrasonic treatment;
(4) adding diethanolamine into the mixed solvent after the ultrasonic treatment, stirring, and dropwise adding ammonia water to adjust the pH value of the solution to obtain stable and uniform sol;
(5) standing and aging the prepared sol at room temperature;
(6) and drying the aged gel in a drying box, grinding the dried gel into fine powder, and calcining the powder in a muffle furnace to obtain PS I metal oxide particles/metal nano particles/PS II metal oxide particles, namely the gas-sensitive film.
In the technical scheme of the application, PS I metal oxide particles/metal nano particles/PS II metal oxide particles are heterogeneous structures with gas-sensitive film structures different from the traditional photo-assisted semiconductor compounding, and by utilizing two-photon excitation and low-resistance ohmic contact of a system interface, the composition of photo-generated electron-hole pairs is inhibited, the sensitivity of the photo-assisted gas sensor is improved, and the semiconductor gas sensor working at room temperature is developed; on the other hand, the demand on photon energy is reduced, and visible light enhancement of gas sensitive response is realized. The method can effectively promote the effective separation of photo-generated charges in the gas-sensitive detection process, and also solves the problem of insufficient oxidation-reduction capability of the traditional heterostructure, so that photo-excited charges are utilized most fully.
The gas-sensitive material system constructed by utilizing the photosynthesis mechanism improves the separation efficiency of photo-generated charges, widens the spectral response range, can effectively increase the surface photo-generated electron concentration of semiconductor oxide, transfers more electrons from the sensitive material to oxygen molecules to form adsorbed oxygen according to a surface space charge layer gas-sensitive mechanism model, further influences the resistance change of the material in the reaction process with target gas, and improves the detection sensitivity and the detection limit.
The preparation method is simple, the raw materials are easy to obtain, and the method is beneficial to large-scale popularization and utilization.
Preferably, the PS I metal oxide precursor solution in the step (1) is an aqueous solution containing at least one of metal ions of titanium, tungsten, tin and zinc, and the molar concentration is 0.01-1 mol/L.
Preferably, the water bath condition in the step (1) is 55-65 ℃, and the stirring time is 1-3 hours.
Preferably, in the step (2), the metal nanoparticle precursor includes silver nitrate, chloroauric acid, and palladium nitrate, the solvent is one of dimethylformamide, ethanol, or ethylene glycol, and the molar ratio of the PS I metal oxide precursor to the metal nanoparticle precursor is 100: 1 to 100: 50.
Preferably, in the step (2), the water bath condition is 55-65 ℃, and the stirring time is 1-3 hours.
Preferably, in the step (3), the molar concentration ratio of the PS I metal oxide precursor to the PS II metal oxide particles is 1: 1-100: 1, the ultrasonic treatment time is 5-10 hours, and the ultrasonic power is 100-500 watts.
Preferably, in the step (4), the amount of the diethanolamine is 1.8-2.2ml, and ammonia water is added dropwise to adjust the pH of the solution to 7.8-8.2.
Preferably, in the step (5), standing and aging are carried out for 70 to 75 hours at room temperature.
Preferably, in the step (6), the drying is carried out in the drying oven for 22-26 hours, the calcination temperature in the muffle furnace is 600-700 ℃, the calcination time is 2-4 hours, and the gas atmosphere for the annealing treatment is air.
A gas sensor prepared by a preparation method of a gas-sensitive film based on a photosynthesis mechanism comprises a polyimide flexible substrate layer, a gold interdigital electrode layer and a gas-sensitive film layer of PS I metal oxide particles/metal nanoparticles/PS II metal oxide particles, which are subjected to hydrophilic treatment, from bottom to top in sequence.
Compared with the prior art, the invention has the beneficial effects that:
(1) the PS I metal oxide particles/metal nano particles/PS II metal oxide particles are heterogeneous structures of which gas-sensitive film structures are different from the traditional photo-assisted semiconductor compounding, and by utilizing two-photon excitation and low-resistance ohmic contact of a system interface, the composition of photo-generated electron-hole pairs is inhibited, the sensitivity of the photo-assisted gas sensor is improved, and the semiconductor gas sensor working at room temperature is developed; on the other hand, the demand on photon energy is reduced, and visible light enhancement of gas-sensitive response is realized;
(2) in the gas-sensitive detection process, the effective separation of photo-generated charges can be effectively promoted, the problem of insufficient oxidation-reduction capability of the traditional heterostructure is solved, and the photo-excited charges are utilized most fully;
(3) the gas-sensitive material system constructed by utilizing a photosynthesis mechanism improves the photoproduction charge separation efficiency and widens the spectral response range, the surface photoproduction electron concentration of semiconductor oxide can be effectively increased, more electrons in the air are transferred from a sensitive material to oxygen molecules to form adsorbed oxygen according to a surface space charge layer gas-sensitive mechanism model, and the resistance change of the material is further influenced in the reaction process with target gas, so that the detection sensitivity and the detection limit are improved;
(4) the preparation method is simple, the raw materials are easy to obtain, and the method is beneficial to large-scale popularization and utilization.
Drawings
FIG. 1 is a schematic diagram of the gas sensing mechanism of a conventional heterojunction semiconductor composite system;
FIG. 2 is a diagram of the mechanism of photosynthesis in nature;
FIG. 3 is a schematic diagram of the gas-sensitive mechanism of the artificial photosynthesis system;
FIG. 4 gas sensitive response of a gas sensor of the present invention to periodic exposure to different concentrations of methyl mercaptan vapor;
FIG. 5 is a schematic view of the mechanism of the gas sensor of the present invention.
Labeled as: the gas sensor comprises a 1-polyimide flexible substrate layer, a 2-gold interdigital electrode layer and a 3-gas-sensitive film layer.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the following detailed description of the present invention is provided with reference to specific embodiments.
Example 1
A preparation method of a gas-sensitive film based on a photosynthesis mechanism comprises the following steps:
(1) stirring a PS I metal oxide precursor in a water bath condition to obtain a PS I metal oxide precursor solution, wherein the PS I metal oxide precursor solution in the step (1) is an aqueous solution containing at least one of metal ions of titanium, tungsten, tin and zinc, and the molar concentration is 0.01 mol/L; stirring for 3 hours at 55 ℃ under the water bath condition;
(2) mixing a metal nanoparticle precursor with the PS I metal oxide precursor solution obtained in the step (1), and stirring under a water bath condition to obtain a mixed solvent; the metal nano-particle precursor comprises silver nitrate, chloroauric acid and palladium nitrate, the solvent is one of dimethylformamide, ethanol or ethylene glycol, and the molar ratio of the PSI metal oxide precursor to the metal nano-particle precursor is 100: 1; stirring for 3 hours at 55 ℃ under the water bath condition;
(3) dispersing PS II metal oxide particles in the mixed solvent obtained in the step (2), stirring under a water bath condition, and then carrying out ultrasonic treatment; the molar concentration ratio of the PS I metal oxide precursor to the PS II metal oxide particles is 1: 1, the ultrasonic treatment time is 5 hours, and the ultrasonic power is 500 watts;
(4) adding diethanolamine into the mixed solvent after the ultrasonic treatment, stirring, and dropwise adding ammonia water to adjust the pH value of the solution to obtain stable and uniform sol; the amount of diethanolamine is 1.8ml, ammonia is dripped to adjust the pH value of the solution to 7.8;
(5) standing and aging the prepared sol at room temperature; standing and aging for 70 hours at room temperature;
(6) and drying the aged gel in a drying box, grinding the dried gel into fine powder, and calcining the fine powder in a muffle furnace to obtain PS I metal oxide particles/metal nano particles/PS II metal oxide particles, namely the gas-sensitive film, wherein the drying is carried out in the drying box for 22 hours, the calcining temperature in the muffle furnace is 700 ℃, the calcining time is 2 hours, and the gas atmosphere of the annealing treatment is air.
A gas sensor prepared by a preparation method of a gas-sensitive film based on a photosynthesis mechanism comprises a polyimide flexible substrate layer 1 subjected to hydrophilic treatment, a gold interdigital electrode layer 2 and a gas-sensitive film layer 3 of metal oxide particles PS I/metal nanoparticles/metal oxide particles PS II from bottom to top in sequence.
Example 2
A preparation method of a gas-sensitive film based on a photosynthesis mechanism comprises the following steps:
(1) stirring a PS I metal oxide precursor in a water bath condition to obtain a PS I metal oxide precursor solution, wherein the PS I metal oxide precursor solution in the step (1) is an aqueous solution containing at least one of metal ions of titanium, tungsten, tin and zinc, and the molar concentration is 0.5 mol/L; the temperature of the water bath is 60 ℃, and the stirring time is 2 hours;
(2) mixing a metal nanoparticle precursor with the PS I metal oxide precursor solution obtained in the step (1), and stirring under a water bath condition to obtain a mixed solvent; the metal nanoparticle precursor comprises silver nitrate, gold fluoacid and palladium nitrate, the solvent is one of dimethylformamide, ethanol or glycol, and the molar ratio of the PS I metal oxide precursor to the metal nanoparticle precursor is 97: 3; the temperature of the water bath is 60 ℃, and the stirring time is 2 hours;
(3) dispersing PS II metal oxide particles in the mixed solvent obtained in the step (2), stirring under a water bath condition, and then carrying out ultrasonic treatment; the molar concentration ratio of the PS I metal oxide precursor to the PS II metal oxide particles is 50: 1, the ultrasonic treatment time is 7 hours, and the ultrasonic power is 300 watts;
(4) adding diethanolamine into the mixed solvent after the ultrasonic treatment, stirring, and dropwise adding ammonia water to adjust the pH value of the solution to obtain stable and uniform sol; the amount of diethanolamine is 2ml, ammonia is dripped to adjust the pH value of the solution to 8;
(5) standing and aging the prepared sol at room temperature; standing and aging for 72 hours at room temperature;
(6) and drying the aged gel in a drying box, grinding the dried gel into fine powder, and calcining the fine powder in a muffle furnace to obtain PS I metal oxide particles/metal nano particles/PS II metal oxide particles, namely the gas-sensitive film, wherein the drying is carried out in the drying box for 24 hours, the calcining temperature in the muffle furnace is 650 ℃, the calcining time is 3 hours, and the gas atmosphere of the annealing treatment is air.
A gas sensor prepared by a preparation method of a gas-sensitive film based on a photosynthesis mechanism comprises a polyimide flexible substrate layer 1 subjected to hydrophilic treatment, a gold interdigital electrode layer 2 and a gas-sensitive film layer 3 of metal oxide particles PS I/metal nanoparticles/metal oxide particles PS II from bottom to top in sequence.
Example 3
A preparation method of a gas-sensitive film based on a photosynthesis mechanism comprises the following steps:
(1) stirring a PS I metal oxide precursor under a water bath condition to obtain a PS I metal oxide precursor solution, wherein the PS I metal oxide precursor solution in the step (1) is an aqueous solution containing at least one of titanium, tungsten, tin and zinc metal ions, and the molar concentration is 1 mol/L; the water bath condition is 65 ℃, and the stirring time is 1 hour;
(2) mixing a metal nanoparticle precursor with the PS I metal oxide precursor solution obtained in the step (1), and stirring under a water bath condition to obtain a mixed solvent; the metal nanoparticle precursor comprises silver nitrate, chloroauric acid and palladium nitrate, the solvent is one of dimethylformamide, ethanol or ethylene glycol, and the molar ratio of the PS I metal oxide precursor to the metal nanoparticle precursor is 100: 50; the water bath condition is 65 ℃, and the stirring time is 1 hour;
(3) dispersing PS II metal oxide particles in the mixed solvent obtained in the step (2), stirring under a water bath condition, and then carrying out ultrasonic treatment; the molar concentration ratio of the PS I metal oxide precursor to the PS II metal oxide particles is 100: 1, the ultrasonic treatment time is 10 hours, and the ultrasonic power is 100 watts;
(4) adding diethanolamine into the mixed solvent after the ultrasonic treatment, stirring, and dropwise adding ammonia water to adjust the pH value of the solution to obtain stable and uniform sol; the amount of diethanolamine is 2.2ml, ammonia is dripped to adjust the pH value of the solution to 8.2;
(5) standing and aging the prepared sol at room temperature; standing and aging for 75 hours at room temperature;
(6) and drying the aged gel in a drying box, grinding the dried gel into fine powder, and calcining the fine powder in a muffle furnace to obtain PS I metal oxide particles/metal nano particles/PS II metal oxide particles, namely the gas-sensitive film, wherein the drying time in the drying box is 26 hours, the calcining temperature in the muffle furnace is 600 ℃, the calcining time is 4 hours, and the gas atmosphere of the annealing treatment is air.
A gas sensor prepared by a preparation method of a gas-sensitive film based on a photosynthesis mechanism comprises a polyimide flexible substrate layer 1 subjected to hydrophilic treatment, a gold interdigital electrode layer 2 and a gas-sensitive film layer 3 of metal oxide particles PS I/metal nanoparticles/metal oxide particles PS II from bottom to top in sequence.
Test examples
Mixing 4.39g C4H6O4Zn·2H2Dispersing O in 60ml of absolute ethyl alcohol, heating in a water bath at the normal pressure of 60 ℃ and stirring for 2 hours to obtain a zinc acetate solution, thus obtaining a zinc oxide precursor solution; 0.10g AgNO3Dispersing in zinc acetate solution, heating in water bath at 60 deg.C under normal pressure, stirring for 2 hr to obtain mixed solution
(2) Dispersing 4.64g of tungsten trioxide in the mixed solution in the step (1), wherein the ultrasonic treatment time is 4 hours, and the ultrasonic power is 200 watts to obtain the mixed solvent;
(3) adding the solvent in the step (2) and 2ml of diethanolamine as a stabilizer, heating and stirring in a water bath at 60 ℃, and dropwise adding ammonia water to adjust the pH value of the solution to 8 to obtain stable and uniform sol;
(4) standing and aging the prepared sol for 72 hours at room temperature;
(5) drying the gel aged in the step (4) in a drying oven for 24 hours, grinding the gel into fine powder, placing the fine powder in a muffle furnace, heating to 200 ℃ (the heating rate is 1 ℃/min), preserving heat for 30min, continuing to heat to 650 ℃, preserving heat for 3 hours, grinding after calcining and naturally cooling to obtain ZnO/Ag/WO3A gas-sensitive composite.
The above-mentioned embodiments only express the specific embodiments of the present application, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present application. It should be noted that, for those skilled in the art, without departing from the technical idea of the present application, several changes and modifications can be made, which are all within the protection scope of the present application.
Claims (10)
1. A preparation method of a gas-sensitive film based on a photosynthesis mechanism is characterized by comprising the following steps:
(1) stirring the PS I metal oxide precursor under the water bath condition to obtain a PS I metal oxide precursor solution;
(2) mixing the metal nano-particle precursor with the PS I metal oxide precursor solution obtained in the step (1), and carrying out water bath
Stirring under a condition to obtain a mixed solvent;
(3) dispersing PS II metal oxide particles in the mixed solvent obtained in the step (2), stirring under a water bath condition, and then carrying out ultrasonic treatment;
(4) adding diethanolamine into the mixed solvent after the ultrasonic treatment, stirring, and dropwise adding ammonia water to adjust the pH value of the solution to obtain stable and uniform sol;
(5) standing and aging the prepared sol at room temperature;
(6) and drying the aged gel in a drying box, grinding the dried gel into fine powder, and calcining the fine powder in a muffle furnace to obtain PSI metal oxide particles/metal nano particles/PS II metal oxide particles, namely the gas-sensitive membrane.
2. The method for preparing a gas-sensitive film based on the photosynthesis mechanism according to claim 1,
in the step (1), the PS I metal oxide precursor solution is an aqueous solution containing at least one of titanium, tungsten, tin and zinc metal ions, and the molar concentration is 0.01-1 mol/L.
3. The method for preparing a gas-sensitive membrane based on a photosynthesis mechanism according to claim 1, wherein the temperature of the water bath in step (1) is 55-65 ℃ and the stirring time is 1-3 hours.
4. The method for preparing a gas-sensitive film based on a photosynthesis mechanism according to claim 1, wherein in the step (2), the metal nanoparticle precursor comprises silver nitrate, chloroauric acid, and palladium nitrate, the solvent is one of dimethylformamide, ethanol, and ethylene glycol, and the molar ratio of the PS I metal oxide precursor to the metal nanoparticle precursor is 100: 1 to 100: 50.
5. The method for preparing a gas-sensitive membrane based on a photosynthesis mechanism according to claim 1, wherein in the step (2), the temperature of the water bath is 55-65 ℃ and the stirring time is 1-3 hours.
6. The method as claimed in claim 1, wherein in step (3), the molar concentration ratio of the PS I metal oxide precursor to the PS II metal oxide particles is 1: 1-100: 1, the sonication time is 5-10 hours, and the sonication power is 100-500W.
7. The method for preparing a gas-sensitive film based on a photosynthesis mechanism according to claim 1, wherein in the step (4), the amount of diethanolamine is 1.8-2.2ml, and ammonia water is added dropwise to adjust the pH of the solution to 7.8-8.2.
8. The method for preparing a gas-sensitive film based on a photosynthesis mechanism according to claim 1, wherein in the step (5), the film is left standing and aged at room temperature for 70-75 hours.
9. The method as claimed in claim 1, wherein in step (6), the gas-sensitive membrane is dried in a drying oven for 22-26 hours, the calcination temperature in the muffle furnace is 600-700 ℃, the calcination time is 2-4 hours, and the annealing treatment is performed in air.
10. A gas sensor manufactured by the method for manufacturing a gas-sensitive film based on a photosynthesis mechanism according to any one of claims 1 to 9, wherein: the gas sensor sequentially comprises a polyimide flexible substrate layer subjected to hydrophilic treatment, a gold interdigital electrode layer and a gas-sensitive film layer of PS I metal oxide particles/metal nanoparticles/PS II metal oxide particles from bottom to top.
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