CN113552295A - Controllable growth lead sulfide composite film gas sensor and preparation method thereof - Google Patents
Controllable growth lead sulfide composite film gas sensor and preparation method thereof Download PDFInfo
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- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 3
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- RWVGQQGBQSJDQV-UHFFFAOYSA-M sodium;3-[[4-[(e)-[4-(4-ethoxyanilino)phenyl]-[4-[ethyl-[(3-sulfonatophenyl)methyl]azaniumylidene]-2-methylcyclohexa-2,5-dien-1-ylidene]methyl]-n-ethyl-3-methylanilino]methyl]benzenesulfonate Chemical compound [Na+].C1=CC(OCC)=CC=C1NC1=CC=C(C(=C2C(=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=2C(=CC(=CC=2)N(CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=C1 RWVGQQGBQSJDQV-UHFFFAOYSA-M 0.000 description 1
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- YZYKBQUWMPUVEN-UHFFFAOYSA-N zafuleptine Chemical compound OC(=O)CCCCCC(C(C)C)NCC1=CC=C(F)C=C1 YZYKBQUWMPUVEN-UHFFFAOYSA-N 0.000 description 1
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
- G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
- G01N33/0037—NOx
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
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- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
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Abstract
The invention provides a controllable growth lead sulfide composite film gas sensor and a preparation method thereof, belonging to the technical field of gas sensing.
Description
Technical Field
The invention belongs to the technical field of gas sensing, and particularly relates to a controllable growth lead sulfide composite film gas sensor and a preparation method thereof.
Background
In the process of industrial production, transportation and the like, a large amount of toxic and harmful gases including nitrogen oxides, carbon oxides, sulfur oxides and the like are emitted. These toxic and harmful gases not only cause environmental problems, but also harm human health. Such as nitrogen dioxide (NO)2) It not only pollutes water, soil and atmosphere, but also is one of main causes of acid rain and photochemical smog, and can cause serious harm to human lung, and cause respiratory system diseases such as emphysema and bronchitis. Therefore, the prepared gas sensor with high sensitivity, good stability and low cost has important application value for an environmental quality detection and early warning system.
The semiconductor gas sensor has the advantages of high sensitivity, simple operation, low cost and the like, but the poor selectivity and high working temperature limit the wide application of the semiconductor gas sensor. As an important narrow-band-gap semiconductor material, the metal sulfide has good application prospect in various fields due to the unique physical and chemical characteristics and the characteristics of low cost, easy preparation and high sensitivity. Lead sulfide is a common direct band gap p-type semiconductor material, is widely applied to the fields of solar cells, infrared detectors and the like, and also shows excellent room-temperature working performance in the field of gas sensors. However, because lead sulfide is difficult to dissolve/disperse in most solvents, a sensitive film with uneven distribution is easily formed by adopting the traditional processes of spin coating, drop coating and the like, and the process stability of the sensor is greatly influenced. The continuous ionic layer adsorption and reaction method (SILAR) is based on heterogeneous reaction between ions adsorbed on a solid-liquid interface and dissolved ions, has the advantages of simple process, controllable process, low synthesis temperature and low cost, and the material prepared by the method has controllable grain size and uniform distribution. The continuous ion layer adsorption and reaction method comprises the specific steps of sequentially soaking the substrate in a stable precursor solution, and washing away unreacted ions on the surface by using deionized water.
However, because the surface of the substrate is smooth, the non-uniform lead sulfide is difficult to be directly synthesized on the surface of the substrate by using a continuous ionic layer adsorption and reaction method, and the gas-sensitive performance of the gas sensor is greatly influenced.
Disclosure of Invention
The invention provides a controllable growth lead sulfide composite film gas sensor and a preparation method thereof aiming at the problems in the prior art, and the controllable uniform growth of lead sulfide is realized and the gas-sensitive performance is improved by synthesizing a transition layer sensitive film on the surface of a substrate.
The technical scheme adopted by the invention is as follows:
a controllable growth lead sulfide composite film gas sensor comprises a substrate, interdigital electrodes prepared on the surface of the substrate and a lead sulfide film synthesized on the surface of the substrate by a continuous ionic layer adsorption and reaction method, and is characterized in that a transition layer sensitive film with adsorption performance on metal ions is arranged between the substrate and the lead sulfide film.
Furthermore, the transition layer sensitive film is made of an n-type semiconductor material, so that a p-n heterojunction can be formed with the lead sulfide film, and the gas-sensitive performance of a single lead sulfide material can be improved.
Furthermore, the material of the transition layer sensitive film is a composite material compounded by one or more of metal oxide, two-dimensional transition metal sulfide or carbon-based material.
Further, the metal oxide is zinc oxide, tin oxide, titanium oxide, or the like, the two-dimensional transition metal sulfide is molybdenum disulfide, tin disulfide, tungsten disulfide, or the like, and the carbon-based material is reduced graphene oxide, or the like.
Furthermore, the thickness of the transition layer sensitive film is 100-200 nm.
Furthermore, the distance between the interdigital electrodes is 100-200 mu m, and the interdigital electrodes are made of gold.
A preparation method of a controllable growth lead sulfide composite film gas sensor is characterized by comprising the following steps:
step 1: cleaning and pretreating a substrate, and then preparing an interdigital electrode on the surface of the substrate;
step 2: preparing a transition layer sensitive film with the adsorption performance on metal ions on the surface of the substrate obtained in the step 1;
and step 3: and (3) synthesizing a lead sulfide film on the surface of the transition layer sensitive film obtained in the step (2) by adopting a continuous ionic layer adsorption and reaction method, and finally preparing the controllable growth lead sulfide composite film gas sensor.
Further, the specific synthesis process of step 3 is as follows: and (3) respectively preparing a lead ion source aqueous solution and a sulfide ion source aqueous solution with plasma concentrations, sequentially immersing the sample obtained in the step (2) into the lead ion source aqueous solution, deionized water, the sulfide ion source aqueous solution and the deionized water for 1min, and performing deposition cycle for multiple times to obtain the lead sulfide film after drying.
Furthermore, the ion concentration range of the lead ion source aqueous solution and the sulfur ion source aqueous solution in the step 3 is 0.001-1 mol/L.
Further, the number of cycles in step 3 is not less than 3.
Further, the drying temperature in the step 3 is in a range of 45-65 ℃.
Furthermore, in the step 1, the distance between the interdigital electrodes is 100-200 μm, and the interdigital electrodes are made of gold.
Further, in the step 2, the transition layer sensitive film is prepared by adopting processes such as spin coating, drop coating, spray coating, electrostatic spinning or screen printing and the like.
Further, the material of the transition layer sensitive film in the step 2 is an n-type semiconductor material.
Further, the material of the transition layer sensitive film in the step 2 is a composite material compounded by one or more of metal oxide, two-dimensional transition metal sulfide or carbon-based material.
Further, the thickness of the transition layer sensitive film in the step 2 is 100-200 nm.
The invention has the beneficial effects that:
1. the invention provides a controllable growth lead sulfide composite film gas sensor and a preparation method thereof.A transition layer sensitive film is prepared on the surface of a substrate, and then a continuous ionic layer adsorption and reaction method is adopted to synthesize a lead sulfide film, so that lead sulfide nano particles are successfully and uniformly and efficiently distributed on the surface of the substrate to obtain the lead sulfide gas sensitive film with controllable grain size;
2. the invention solves the problem that the lead sulfide nano-particles are difficult to grow on the surface of the smooth substrate, and the prepared gas sensor has high response, good stability and low cost and is suitable for large-scale production;
3. preferably, when the n-type semiconductor material is used as the transition layer sensitive film, the transition layer sensitive film and the lead sulfide film can form a p-n heterojunction, so that the gas-sensitive performance of the lead sulfide single material is improved.
Drawings
FIG. 1 is a schematic structural diagram of a controllable growth lead sulfide composite thin film gas sensor obtained in example 1 of the present invention;
FIG. 2 is a comparative scanning electron micrograph of a zinc oxide/lead sulfide thin film obtained in example 1 of the present invention and a lead sulfide thin film obtained in a comparative example, wherein (a) is a zinc oxide/lead sulfide thin film and (b) is a lead sulfide thin film;
FIG. 3 shows NO of the controlled growth lead sulfide composite thin film gas sensor obtained in example 1 of the present invention2A dynamic response test pattern;
FIG. 4 is a graph showing the repeatability of a gas sensor with a controlled growth of a lead sulfide composite thin film obtained in example 1 of the present invention;
FIG. 5 shows NO of lead sulfide thin film gas sensor obtained in comparative example of the present invention2A dynamic response test pattern.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described with reference to the following embodiments and the accompanying drawings.
Example 1
The embodiment provides a controllable growth lead sulfide composite film gas sensor, which comprises a flexible substrate, a transition layer sensitive film and a lead sulfide film, wherein the flexible substrate, the transition layer sensitive film and the lead sulfide film are sequentially arranged from bottom to top, gold interdigital electrodes with a spacing of 200 mu m are prepared on the surface of the flexible substrate, the transition layer sensitive film is a zinc oxide film, and the thickness of the transition layer sensitive film is about 100 nm.
The embodiment also provides a preparation method of the controllable growth lead sulfide composite film gas sensor, which specifically comprises the following steps:
step 1: cleaning and pretreating a Polyimide (PI) flexible substrate, and then preparing gold interdigital electrodes with the spacing of 200 mu m on the surface of the flexible substrate;
step 2: preparing a zinc oxide precursor film on the surface of the flexible substrate obtained in the step 1, specifically: with zinc acetate dihydrate (Zn (CH)3COO)2·2H2O) as precursor and 2-methoxy ethanol (C)3H8O2) Monoethanolamine (C) as main solvent2H7NO) as stabilizer with a reaction solution in which Zn (CH)3COO)2·2H2O and C2H7The concentration of NO is 0.75 mol/L; stirring the prepared reaction solution at 60 ℃ for 30min, and cooling to room temperature to obtain a sol solution; dropwise adding a small drop of sol solution to the surface of the flexible substrate obtained in the step 1, spin-coating at the rotating speed of 4000rpm for 30s, drying at the temperature of 200 ℃ for 15min, and repeating the spin-coating and drying processes for 3 times to obtain a uniform zinc oxide precursor film;
and step 3: putting the zinc oxide precursor film obtained in the step 2 into a high-temperature furnace at the temperature of 300 ℃ for annealing for 1h to obtain a zinc oxide transition layer film;
and 4, step 4: adopting a continuous ionic layer adsorption and reaction method to synthesize the lead sulfide film on the surface of the zinc oxide transition layer film obtained in the step 3, which specifically comprises the following steps: respectively preparing a lead nitrate aqueous solution and a sodium sulfide aqueous solution with the ion concentration of 0.01mol/L, sequentially immersing the sample obtained in the step 3 into the lead nitrate aqueous solution, the deionized water, the sodium sulfide aqueous solution and the deionized water for 1min, respectively, taking the immersion as a deposition cycle, circulating for 5 times, and drying on a 60 ℃ hot bench to obtain the lead sulfide film. Finally, the controllable growth lead sulfide composite film gas sensor is prepared.
Scanning electron microscope tests are carried out on the controllable growth lead sulfide composite film gas sensor obtained in the embodiment, and the results are shown in fig. 2(a), it can be found that a film formed by uniformly dispersed lead sulfide nano-particles is attached to the surface of the flexible substrate, the grain size of the film is 30-50 nm, and no obvious agglomeration phenomenon exists, which indicates that the preparation method provided by the embodiment can be used for obtaining the lead sulfide gas-sensitive film with controllable and uniform grain size.
The controllable growth lead sulfide composite film gas sensor obtained in the embodiment is put into NO2And measuring the resistance value in the test system, and judging the performance of the sensor according to the change of the resistance value. Introducing air, keeping the humidity at 60% RH, and introducing 10ppm NO after the sensor is stabilized2The gas is aged for several times for one time, after the response results of the sensors are basically consistent, the dynamic response test of the sensors is started, and NO with the concentration of 0.5ppm, 1ppm, 2ppm, 4ppm, 6ppm, 8ppm and 10ppm is introduced in sequence2A gas. NO by the sensor shown in FIG. 32As can be seen from the dynamic response test chart and the repeated performance test chart shown in FIG. 4, the controllable growth lead sulfide composite thin film gas sensor obtained in the embodiment is used for 0.5-10 ppm of NO2All have excellent resolving power and good repeatability.
Example 2
The embodiment provides a controllable growth lead sulfide composite film gas sensor, which comprises a flexible substrate, a transition layer sensitive film and a lead sulfide film from bottom to top, wherein gold interdigital electrodes with the spacing of 200 mu m are prepared on the surface of the flexible substrate, and the transition layer sensitive film is molybdenum disulfide (MoS)2) And the thickness of the film is about 200 nm.
The embodiment also provides a preparation method of the controllable growth lead sulfide composite film gas sensor, which specifically comprises the following steps:
step 1: cleaning and pretreating a Polyimide (PI) flexible substrate, and then preparing gold interdigital electrodes with the spacing of 200 mu m on the surface of the flexible substrate;
step 2: preparing a molybdenum disulfide film on the surface of the flexible substrate obtained in the step 1, specifically: 0.4mmol of sodium molybdate dihydrate (Na) was weighed2MoO4·2H2O) and 1mmol of thioacetamide (CH)3CSNH2) Dissolving in 30ml deionized water, stirring for 20min, transferring the obtained solution to autoclave with polytetrafluoroethylene lining, and autoclaveAfter keeping at 200 ℃ for 36h, taking out and cooling to room temperature; centrifugally cleaning the obtained product with deionized water for several times, and drying at 60 ℃ for 12 hours to obtain molybdenum disulfide nano particles; preparing the obtained molybdenum disulfide nano particles into 1mg/mL aqueous solution, spin-coating the surface of the flexible substrate obtained in the step 1 at the rotating speed of 2000rpm for 30s, drying at 200 ℃ for 15min, and repeating the spin-coating and drying processes for 3 times to obtain a uniform molybdenum disulfide film;
and step 3: adopting a continuous ionic layer adsorption and reaction method to synthesize the lead sulfide film on the surface of the molybdenum disulfide film obtained in the step 2, which specifically comprises the following steps: respectively preparing a lead nitrate aqueous solution and a sodium sulfide aqueous solution with the ion concentration of 0.01mol/L, sequentially immersing the sample obtained in the step 2 into the lead nitrate aqueous solution, the deionized water, the sodium sulfide aqueous solution and the deionized water for 1min, respectively, taking the immersion as a deposition cycle, circulating for 5 times, and drying on a 60 ℃ hot bench to obtain the lead sulfide film. Finally, the controllable growth lead sulfide composite film gas sensor is prepared.
Comparative example
The comparison example provides a lead sulfide film gas sensor which comprises a flexible substrate and a lead sulfide film from bottom to top in sequence, wherein gold interdigital electrodes with the spacing of 200 mu m are prepared on the surface of the flexible substrate.
Compared with the example 1, the method for preparing the lead sulfide thin film gas sensor is only different from the method for preparing the lead sulfide thin film gas sensor in the example 1 in that the steps 2 and 3 for preparing the zinc oxide transition layer thin film are omitted, and the rest steps are unchanged.
Scanning electron microscope test is carried out on the obtained lead sulfide film gas sensor, and the result is shown in fig. 2(b), so that the surface of the flexible substrate is very smooth, which indicates that no obvious lead sulfide gas-sensitive material is attached to the surface of the sensor. The resistance value was measured in the same manner as in example 1 to obtain NO of the sensor shown in FIG. 52And (3) a dynamic response test chart shows that the reference resistance of the sensor is approximately infinite and has no gas-sensitive performance, which shows that the lead sulfide gas-sensitive material is not obviously attached to the surface of the sensor, so that the gas-sensitive performance is not available.
Claims (9)
1. A controllable growth lead sulfide composite film gas sensor comprises a substrate, interdigital electrodes prepared on the surface of the substrate and a lead sulfide film synthesized on the surface of the substrate by a continuous ionic layer adsorption and reaction method, and is characterized in that a transition layer sensitive film with adsorption performance on metal ions is arranged between the substrate and the lead sulfide film.
2. The controlled growth lead sulfide composite thin film gas sensor according to claim 1, wherein the material of the transition layer sensitive thin film is an n-type semiconductor material.
3. The controllable growth lead sulfide composite film gas sensor according to claim 1, wherein the material of the transition layer sensitive film is a composite material compounded by one or more of metal oxide, two-dimensional transition metal sulfide or carbon-based material.
4. The controllable growth lead sulfide composite thin film gas sensor according to claim 1, wherein the thickness of the transition layer sensitive thin film is 100-200 nm.
5. A preparation method of the controllable growth lead sulfide composite film gas sensor as claimed in any one of claims 1 to 4, characterized by comprising the following steps:
step 1: cleaning and pretreating a substrate, and then preparing an interdigital electrode on the surface of the substrate;
step 2: preparing a transition layer sensitive film with the adsorption performance on metal ions on the surface of the substrate obtained in the step 1;
and step 3: and (3) synthesizing a lead sulfide film on the surface of the transition layer sensitive film obtained in the step (2) by adopting a continuous ionic layer adsorption and reaction method, and finally preparing the controllable growth lead sulfide composite film gas sensor.
6. The method for preparing the controllable growth lead sulfide composite film gas sensor according to claim 5, wherein the synthesis process of the step 3 is as follows: and (3) respectively preparing a lead ion source aqueous solution and a sulfide ion source aqueous solution with plasma concentrations, sequentially immersing the sample obtained in the step (2) into the lead ion source aqueous solution, deionized water, the sulfide ion source aqueous solution and the deionized water for 1min, and performing deposition cycle for multiple times to obtain the lead sulfide film after drying.
7. The method for preparing the controllable growth lead sulfide composite film gas sensor according to claim 6, wherein the ion concentration range of the lead ion source aqueous solution and the sulfide ion source aqueous solution in the step 3 is 0.001-1 mol/L.
8. The method for preparing the controllable growth lead sulfide composite film gas sensor according to claim 6, wherein the number of cycles in the step 3 is not less than 3.
9. The method for preparing the controllable growth lead sulfide composite film gas sensor according to claim 5, wherein the transition layer sensitive film is prepared by adopting spin coating, drop coating, spray coating, electrostatic spinning or screen printing in the step 2.
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