CN117705896A - Flexible NO 2 Preparation method of gas sensor and sensor - Google Patents
Flexible NO 2 Preparation method of gas sensor and sensor Download PDFInfo
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- CN117705896A CN117705896A CN202410153354.3A CN202410153354A CN117705896A CN 117705896 A CN117705896 A CN 117705896A CN 202410153354 A CN202410153354 A CN 202410153354A CN 117705896 A CN117705896 A CN 117705896A
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/08—Sulfides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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- Chemical & Material Sciences (AREA)
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- Nanotechnology (AREA)
- Organic Chemistry (AREA)
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- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Molecular Biology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
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- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention relates to a flexible NO 2 A preparation method of a gas sensor and the sensor, wherein the method comprises the following steps: step 1: preparing MoS by adopting a one-step hydrothermal method 2 ZnS composite; step 2: selecting a flexible substrate, and preparing interdigital electrodes on the flexible substrate; step 3: by MoS 2 Preparation of MoS on interdigital electrode 2 ZnS composite film to obtain NO 2 A gas sensor. Flexible NO of the present invention 2 Preparation method of gas sensor, sensor and MoS 2 Preparing NO on flexible substrate by using ZnS composite material as sensitive material 2 Gas sensor, the flexible sensor being sensitive to NO at room temperature 2 The device has good stability and selectivity, low cost and small volume, and is beneficial to being integrated on wearable flexible equipment.
Description
Technical Field
The invention belongs to the technical field of gas sensors, and particularly relates to a flexible NO 2 A method for manufacturing a gas sensor and a sensor are provided.
Background
NO 2 Is a gas which is reddish brown, has pungent smell and has great harm to human body. There are some studies showing that NO is at a certain concentration 2 Serious diseases such as respiratory diseases, cardiovascular diseases, nervous system injury and the like can be caused in the environment. There are many works today that come into contact with NO 2 Gases such as fossil fuel plants, blasting, nuclear waste collection, etc., can put workers at risk for NO 2 In the environment. Thus, NO in working environment or living environment 2 It is important to perform the detection.
Spectrophotometry is the NO in the atmosphere 2 One of the common methods for indirect detection is based on the principle that NO in the atmosphere 2 Absorbing the dye into an absorption bottle, carrying out diazotization reaction with sulfanilic acid, and then carrying out reaction with naphthalene ethylenediamine hydrochloride to generate rose azo dye. The absorbance of the sample was measured at 540 nm using a spectrophotometer, due to the magnitude of the absorbance and the NO in the sample 2 The concentration is proportional to calculate NO in the atmosphere 2 Concentration.
NO in atmosphere 2 The direct measurement method of the concentration mainly comprises a laser induced fluorescence method, a cavity ring-down spectroscopy technology, a differential absorption spectroscopy method and the like. The laser-induced fluorescence method detection mechanism is to utilize laser with specific wavelength to make NO 2 Excited to an excited state, and then collecting NO 2 Molecular de-excitation fluorescent signal, and NO is judged by using fluorescence intensity 2 Concentration. Cavity ring-down spectroscopy was applied to atmospheric NO only in the last decade 2 A method for detecting is to analyze the ring-down time of light reflected in the ring-down cavity for multiple times to obtain the concentration information of the gas to be detected in the cavity. The technology has the advantages of simple measurement, high sensitivity and difficult influence of other interference gases. The differential absorption spectrometry is a common atmosphere monitoring technology, the technology is mainly based on Lambert-Beer law, light attenuation is formed by narrow-band absorption through a filtering technology, then the light attenuation is fitted with a standard reference spectrum by a least square method, and finally the concentration of detected gas can be determined by an inversion method.
Although the selectivity is better, the direct monitoring or the indirect monitoring is not suitable for developing portable NO because of the high cost, large size and not easy integration on mobile equipment 2 And (5) monitoring the instrument. In addition, many hand-held instruments developed at present are rigid gas sensors, which need to work at high temperature (more than or equal to 200 ℃), and for some people doing special work, the high temperature may cause explosion.
Disclosure of Invention
In order to solve the above problems in the prior art, the present invention provides a flexible NO 2 A method for manufacturing a gas sensor and a sensor are provided. The technical problems to be solved by the invention are realized by the following technical scheme:
the invention provides a flexible NO 2 A method of making a gas sensor comprising:
step 1: preparing MoS by adopting a one-step hydrothermal method 2 ZnS composite;
step 2: selecting a flexible substrate, and preparing interdigital electrodes on the flexible substrate;
step 3: by using the MoS 2 Preparation of MoS on the interdigital electrode 2 ZnS composite film to obtain NO 2 A gas sensor.
In one embodiment of the present invention, the step 1 includes:
step 1.1: dissolving ammonium molybdate tetrahydrate, thioacetamide and sodium dodecyl benzene sulfonate in deionized water to obtain a first mixed solution;
step 1.2: zinc acetate dihydrate is added into the first mixed solution, and the solution is stirred at room temperature until the zinc acetate dihydrate is dissolved to obtain a second mixed solution;
step 1.3: transferring the second mixed solution into a stainless steel autoclave with a Teflon lining, and placing the stainless steel autoclave with the second mixed solution into an oven for heating and reacting;
step 1.4: alternately cleaning the reacted product by using deionized water and ethanol, and drying the cleaned product in a vacuum drying oven;
step 1.5: placing the dried product in a muffle furnace, and calcining and annealing in a nitrogen environment to obtain MoS 2 ZnS composite.
In one embodiment of the invention, in the step 1.1, the mass ratio of the ammonium molybdate tetrahydrate, the thioacetamide and the sodium dodecyl benzene sulfonate is (2-4): 6:2.
In one embodiment of the present invention, in the step 1.2, the mass ratio of the added amount of zinc acetate dihydrate to the ammonium molybdate tetrahydrate in the first mixed solution is 15 (20-22).
In one embodiment of the present invention, in the step 1.3, the heating temperature of the oven is 180-200 ℃ and the heating time is 12-24 hours.
In one embodiment of the present invention, in the step 1.4, the drying temperature of the vacuum drying oven is 60 ℃ and the drying time is 12 h.
In one embodiment of the present invention, in the step 1.5, the process parameters of the calcination annealing are: the annealing temperature is 600-800 ℃, the heating rate is 2-5 ℃/min, and the annealing time is 30-60 min.
In one embodiment of the invention, the flexible substrate comprises a PET substrate, a PDMS substrate, a PI substrate, or a PEN substrate.
In one embodiment of the present invention, the step 3 includes:
by using the MoS 2 Forming MoS on the interdigital electrode by PVD, coating, spin coating or CVD process 2 ZnS composite film to obtain NO 2 A gas sensor.
The invention provides a flexible NO 2 A gas sensor prepared by the method of any of the embodiments described above.
Compared with the prior art, the invention has the beneficial effects that:
1. flexible NO of the present invention 2 The preparation method of the gas sensor comprises the steps of firstly preparing MoS through a one-step hydrothermal method 2 ZnS composite material and then use the MoS 2 Preparing NO on flexible substrate by using ZnS composite material as sensitive material 2 A gas sensor. Due to MoS 2 The difference in fermi level with ZnS, when two materials are in contact, the majority charge carriers diffuse causing the incorporation of electron holes, so that the interface where the two materials are in contact forms an immovable charge region, called a depletion layer. When flexible NO 2 The gas sensor being exposed to the target gas, NO 2 Suction MoS 2 Electrons of the/ZnS composite material cause an increase in the hole concentration, so that the carrier concentration is no longer in dynamic equilibrium, and the depletion layer width decreases after transfer of charge, so that the resistance further decreases. When flexible NO 2 After the gas sensor is exposed to the air again, NO 2 Gas separation MoS 2 ZnS composite material, so that electrons return to MoS again 2 The resistance of the ZnS composite material is increased, and NO can be calculated according to a sensitivity formula 2 Is of the concentration of MoS with heterojunction 2 the/ZnS composite will improve the response to some extent;
2. flexible NO of the present invention 2 Method for manufacturing gas sensor by MoS 2 Preparing NO on flexible substrate by using ZnS composite material as sensitive material 2 Gas sensor due to MoS 2 The ZnS composite material has MoS 2 Band gap is adjustable, carrier mobility is high, so that NO is available at room temperature without other external excitation 2 The gas sensor may also haveHas good response and the MoS at room temperature 2 The ZnS composite material is not easy to oxidize, so MoS is used 2 Flexible gas sensor prepared from ZnS composite material for NO at room temperature 2 The catalyst has good stability and selectivity;
3. flexible NO of the present invention 2 Preparation method of gas sensor, on one hand, flexible substrate is adopted, and on the other hand MoS 2 The ZnS composite material has higher effective Young modulus value, so the NO prepared 2 The gas sensor can perform bending test on NO 2 Shows good stability, can be integrated on wearable flexible equipment, and the preparation cost is low and the volume is small.
Drawings
FIG. 1 is a schematic illustration of a flexible NO provided by an embodiment of the invention 2 A flow chart of a method of manufacturing a gas sensor;
FIG. 2 is a MoS provided in an embodiment of the invention 2 X-ray diffraction pattern of ZnS composite;
FIG. 3 is a pure MoS 2 And MoS 2 Scanning electron microscope image of ZnS composite, wherein (a) image is pure MoS 2 Namely, S0 and (b) are the MoS of example 1 2 Scanning electron microscope image of ZnS composite, namely S1;
FIG. 4 is a graph of NO produced in each of example 1 and comparative example provided in the examples of the present invention 2 Gas sensor for 100ppm NO at room temperature 2 Is a test graph of (2);
FIG. 5 is a sample of NO produced in example 1 provided in the examples of the present invention 2 The gas sensor is sensitive to NO in an air detection background at room temperature 2 Response recovery time profile of (2);
FIG. 6 is a graph of NO produced in example 1 provided in the examples of the present invention 2 The gas sensor is suitable for NO with different concentrations at room temperature 2 A response value change curve and a fitting curve, wherein (a) the graph is NO prepared in example 1 2 The gas sensor is suitable for NO with different concentrations at room temperature 2 And (b) is a graph of the response value change of NO prepared in example 1 2 The gas sensor is suitable for NO with different concentrations at room temperature 2 A fitted curve of response values and concentration;
FIG. 7 is a graph of NO produced in each of example 1 and comparative example provided in the examples of the present invention 2 A histogram of response values of the gas sensor to different types of detection gases at room temperature;
FIG. 8 is a graph of NO produced in example 1 provided in the examples of the present invention 2 Gas sensor for 100ppm NO at room temperature 2 Is a seven cycle test plot of (2);
FIG. 9 is a graph of NO produced in each of example 1 and comparative example provided in the examples of the present invention 2 Gas sensor for 100ppm NO at room temperature 2 Is a comparison of the time stability response of (2);
FIG. 10 is a sample of NO produced in example 1 provided in the examples of the present invention 2 The gas sensor is sensitive to 100ppm NO at different bending degrees at room temperature 2 A response value variation graph of (a);
FIG. 11 is a graph of NO produced in example 1 provided in the examples of the present invention 2 The gas sensor was subjected to 100ppm NO after 500 cycles of bending-relaxation at different curvatures at room temperature 2 A response value variation graph of (a).
Detailed Description
In a first aspect, embodiments of the present invention provide a flexible NO 2 Referring to fig. 1, fig. 1 is a schematic diagram showing a method for manufacturing a gas sensor according to an embodiment of the present invention 2 A flow chart of a method for manufacturing a gas sensor is shown in FIG. 1, and the flexible NO of the embodiment 2 A method of making a gas sensor comprising:
step 1: preparing MoS by adopting a one-step hydrothermal method 2 ZnS composite.
In an alternative embodiment, step 1 includes:
step 1.1: will (NH) 4 ) 6 Mo 7 O 24 ·4H 2 O (ammonium molybdate tetrahydrate), C 2 H 5 NS (thioacetamide) and SDBS (sodium dodecyl benzene sulfonate) were dissolved in deionized water to obtain a first mixed solution.
Optionally, (NH) 4 ) 6 Mo 7 O 24 ·4H 2 O、C 2 H 5 The mass ratio of NS to SDBS is (2-4) 6:2.
Step 1.2: c is C 4 H 6 O 4 Zn·2H 2 O (zinc acetate dihydrate) was added to the first mixed solution and stirred at room temperature until dissolved to give a second mixed solution.
Alternatively, C 4 H 6 O 4 Zn·2H 2 The mass ratio of the addition amount of O to the ammonium molybdate tetrahydrate in the first mixed solution is 15 (20-22).
Step 1.3: the second mixed solution was transferred to a teflon lined stainless steel autoclave, which was heated in an oven to react.
Optionally, the heating temperature of the oven is 180-200 ℃ and the heating time is 12-24 hours.
Step 1.4: and alternately cleaning the reacted product by using deionized water and ethanol, and drying the cleaned product in a vacuum drying oven.
Alternatively, the reacted product may be alternately washed 3 times with deionized water and ethanol. The drying temperature of the vacuum drying oven is 60 ℃ and the drying time is 12 h.
Step 1.5: placing the dried product in a muffle furnace, and calcining and annealing in a nitrogen environment to obtain MoS 2 ZnS composite.
Optionally, the process parameters of calcination annealing are: the annealing temperature is 600-800 ℃, the heating rate is 2-5 ℃/min, and the annealing time is 30-60 min.
Step 2: and selecting a flexible substrate, and preparing interdigital electrodes on the flexible substrate.
Alternatively, the flexible substrate may be a PET (polyethylene terephthalate) substrate, a PDMS (polydimethylsiloxane) substrate, a PI (polyimide) substrate, or a PEN (polyethylene naphthalate) substrate. The interdigital electrode may be a silver interdigital electrode.
In this embodiment, the surface of the selected flexible substrate may be plasma treated to increase the roughness of the surface, and then silver interdigital electrodes may be printed on the surface of the plasma treated PET substrate using an inkjet printer.
Step 3: by MoS 2 Preparation of MoS on interdigital electrode 2 ZnS composite film to obtain NO 2 A gas sensor.
Alternatively, moS may be prepared on the interdigitated electrodes by PVD (Physical Vapor Deposition ), coating, spin coating, or CVD (Chemical Vapor Deposition ) processes 2 ZnS composite film to obtain NO 2 A gas sensor.
Taking PVD process as an example, 5-10 mg MoS is weighed 2 The ZnS composite material is dispersed in 0.75-1.5 ml DI (deionized water), the mixed solution is placed in an ultrasonic machine for ultrasonic treatment for 1-2 min, the uniformly mixed solution is placed in a PVD liquid container, and MoS is deposited on an interdigital electrode 2 Wet film of/ZnS, finally comprising MoS 2 Placing the ZnS wet film substrate in a vacuum drying oven at 60deg.C for 12 hr to obtain NO 2 A gas sensor.
Flexible NO according to embodiments of the invention 2 The preparation method of the gas sensor comprises the steps of firstly preparing MoS through a one-step hydrothermal method 2 ZnS composite material and then use the MoS 2 Preparing NO on flexible substrate by using ZnS composite material as sensitive material 2 A gas sensor. Due to MoS 2 The difference in fermi level with ZnS, when two materials are in contact, the majority charge carriers diffuse causing the incorporation of electron holes, so that the interface where the two materials are in contact forms an immovable charge region, called a depletion layer. When flexible NO 2 The gas sensor being exposed to the target gas, NO 2 Suction MoS 2 Electrons of the/ZnS composite material cause an increase in the hole concentration, so that the carrier concentration is no longer in dynamic equilibrium, and the depletion layer width decreases after transfer of charge, so that the resistance further decreases. When flexible NO 2 After the gas sensor is exposed to the air again, NO 2 Gas separation MoS 2 ZnS composite material, so that electrons return to MoS again 2 ZnS composite material and resistorIncreasing, and calculating according to the sensitivity formula to obtain NO 2 Is of the concentration of MoS with heterojunction 2 the/ZnS composite will improve the response to some extent.
Second, due to MoS 2 The ZnS composite material has MoS 2 Band gap is adjustable, carrier mobility is high, so that NO is available at room temperature without other external excitation 2 The gas sensor can also have good response, and the MoS at room temperature 2 The ZnS composite material is not easy to oxidize, so MoS 2 Flexible gas sensor prepared from ZnS composite material for NO at room temperature 2 Has good stability and selectivity. Furthermore, in the flexible NO of the present embodiment 2 In the preparation method of the gas sensor, a flexible substrate is adopted on one hand, and MoS on the other hand 2 The ZnS composite material has higher effective Young modulus value, so the NO prepared 2 The gas sensor can perform bending test on NO 2 Exhibit good stability and can also be integrated on wearable flexible devices.
In a second aspect, embodiments of the present invention provide a flexible NO 2 Gas sensor, the flexible NO 2 Gas sensor utilizing the flexible NO provided in the first aspect 2 The gas sensor is prepared by the preparation method. In particular, the flexible NO 2 The gas sensor comprises a flexible substrate, interdigital electrodes and MoS arranged from bottom to top 2 ZnS composite film.
With respect to the flexible NO 2 Details of the gas sensor and corresponding advantageous effects, please refer to the flexible NO provided in the first aspect 2 The relevant content of the preparation method of the gas sensor is not described herein.
Further, the flexible NO of the present invention is exemplified by 2 Method for preparing gas sensor, and sensor and effect are described in detail, wherein MoS is prepared 2 In the process of the ZnS composite, (NH) 4 ) 6 Mo 7 O 24 ·4H 2 O、C 2 H 5 The mass ratio of NS to SDBS is 3:6:2.
Example 1
Step a: weigh 0.62. 0.62 g (NH) 4 ) 6 Mo 7 O 24 ·4H 2 O，1.2g C 2 H 5 NS and 0.4g SDBS were dispersed in 60 mL deionized water and stirred at room temperature until fully dissolved to give a first mixed solution;
step b: weigh 3.5 mmol C 4 H 6 O 4 Zn·2H 2 Dispersing O in the uniformly stirred first mixed solution in the step a, and stirring at room temperature until the O is fully dissolved to obtain a second mixed solution;
step c: transferring the second mixed solution obtained in the step b into a stainless steel autoclave with a Teflon lining of 100 ml, and heating the second mixed solution in an oven at 180 ℃ for 24 h to react;
step d: after the second mixed solution is completely reacted, alternately cleaning the reaction product for three times by using deionized water and ethanol, and finally drying 12 h in a vacuum drying oven at 60 ℃;
step e: placing the dried product in a muffle furnace, calcining and annealing for 60 min at 700 ℃ in a nitrogen environment, wherein the heating rate is 5 ℃/min, and obtaining MoS after the calcining and annealing are completed 2 ZnS composite;
step f: carrying out plasma treatment on the surface of the PET substrate to increase the surface roughness, and then printing silver interdigital electrodes on the surface of the PET substrate subjected to the plasma treatment by using an ink-jet printer;
step g: weighing MoS in step e of 5 mg 2 Dispersing ZnS composite material in DI of 1.5 ml, placing the mixed solution in an ultrasonic machine for ultrasonic treatment for 2 min, placing the uniformly mixed solution in PVD liquid container, and depositing on silver interdigital electrode to obtain MoS 2 Wet film of/ZnS, finally comprising MoS 2 Placing the ZnS wet film substrate in a vacuum drying oven at 60deg.C for 12 hr to obtain NO 2 A gas sensor.
Example 2
Step a: weigh 0.62. 0.62 g (NH) 4 ) 6 Mo 7 O 24 ·4H 2 O，1.2g C 2 H 5 NS and 0.4g SDBS were dispersed in 60 mL deionized waterStirring at room temperature until the mixture is fully dissolved to obtain a first mixed solution;
step b: weigh 4 mmol C 4 H 6 O 4 Zn·2H 2 Dispersing O in the uniformly stirred first mixed solution in the step a, and stirring at room temperature until the O is fully dissolved to obtain a second mixed solution;
step c: transferring the second mixed solution obtained in the step b into a stainless steel autoclave with a Teflon lining of 100 ml, and heating the second mixed solution in an oven at 180 ℃ for 24 h to react;
step d: after the second mixed solution is completely reacted, alternately cleaning the reaction product for three times by using deionized water and ethanol, and finally drying 12 h in a vacuum drying oven at 60 ℃;
step e: placing the dried product in a muffle furnace, calcining and annealing for 60 min at 700 ℃ in a nitrogen environment, wherein the heating rate is 5 ℃/min, and obtaining MoS after the calcining and annealing are completed 2 ZnS composite;
step f: carrying out plasma treatment on the surface of the PET substrate to increase the surface roughness, and then printing silver interdigital electrodes on the surface of the PET substrate subjected to the plasma treatment by using an ink-jet printer;
step g: weighing MoS in step e of 5 mg 2 Dispersing ZnS composite material in DI of 1.5 ml, placing the mixed solution in an ultrasonic machine for ultrasonic treatment for 2 min, placing the uniformly mixed solution in PVD liquid container, and depositing on silver interdigital electrode to obtain MoS 2 Wet film of/ZnS, finally comprising MoS 2 Placing the ZnS wet film substrate in a vacuum drying oven at 60deg.C for 12 hr to obtain NO 2 A gas sensor.
Comparative example
Step a: obtaining pure MoS 2 A material;
it will be appreciated that pure MoS 2 The material can be a product sold in the market or prepared by using related raw materials.
Step b: carrying out plasma treatment on the surface of the PET substrate to increase the surface roughness, and then printing silver interdigital electrodes on the surface of the PET substrate subjected to the plasma treatment by using an ink-jet printer;
step c: weigh 5 mg pure MoS 2 Dispersing the material in DI of 1.5 ml, placing the mixed solution in an ultrasonic machine for ultrasonic treatment for 2 min, placing the uniformly mixed solution in a PVD liquid container, and depositing on silver interdigital electrode to obtain MoS 2 Wet film, finally will contain MoS 2 Placing the wet film substrate in a vacuum drying oven at 60deg.C for 12 hr to obtain NO 2 A gas sensor.
Further, for the MoS of example 1 2 The ZnS composite is denoted as S1 and NO prepared by using the same 2 The gas sensor is designated as M1, pure MoS of comparative example 2 The material is marked as S0 and NO prepared by using the same 2 The gas sensor is marked as M0, and analysis and test are respectively carried out, wherein, a Fluke 8846a high-precision digital multimeter is used for measuring NO 2 Resistance value of the gas sensor.
Referring to FIG. 2, FIG. 2 is a MoS provided in an embodiment of the invention 2 As can be seen from FIG. 2, each peak of sample S1 corresponds to a hexagonal phase 2H-MoS, respectively 2 (JCPDS No. 37-1492) and ZnS (JCPDS No. 1-792) can observe the corresponding MoS in S1 2 (002) And (100) peak was attenuated, possibly because ZnS growth inhibited MoS 2 (002) And (100) crystal plane growth such that MoS 2 The crystallinity of (c) becomes poor.
Referring to FIG. 3, FIG. 3 is a pure MoS 2 And MoS 2 Scanning electron microscope image of ZnS composite, wherein the image (a) in FIG. 3 is pure MoS 2 Namely, S0 and (b) are the MoS of example 1 2 Scanning electron microscopy of ZnS composite, S1, by which it can be seen that both samples are nanoflower shaped, pure MoS in (a) figure 2 The nanoplates were smooth, while (b) MoS in the plot 2 The surface roughness of the/ZnS composite also indicates the formation of MoS 2 ZnS composite.
Referring to FIG. 4, FIG. 4 shows the NO produced in each of example 1 and comparative example provided in the examples of the present invention 2 Gas sensor for 100ppm NO at room temperature 2 A graph of Response value (Response) versus Time (Time). Wherein the sensor is transferred to the air with the resistance remaining stable and the resistance is marked as Ra and the sensor is transferred to 100ppm NO 2 Is marked as Rg when the resistance is stable; the sensor is transferred to the air, and the resistance gradually recovers to Ra; sensor for NO 2 Is calculated according to the formula s=ra/Rg. According to the test analysis, the gas-sensitive performance of the sensor M1 is superior to that of the sensor M0, and one of the main reasons is that the heterojunction formed in the sample S1 greatly improves the transfer of electron holes. Sensor with sample S1 as gas sensitive material for NO at room temperature 2 The response of (c) reaches the highest, s=335%.
Referring to FIG. 5, FIG. 5 shows the NO produced in example 1 according to the present invention 2 The gas sensor is sensitive to NO in an air detection background at room temperature 2 Response recovery time profile of (a). Wherein the response Time and recovery Time of the sensor are calculated from the response of the sensor to acetone and the Time (Time) required for the recovery phase to reach 90% change in Resistance (Resistance). The calculation result shows that the response of the sensor M1 to acetone is only 8s, and the recovery time is 120s, which shows that the sensor M1 can realize the reaction to NO 2 Is provided.
Referring to FIG. 6, FIG. 6 shows the NO produced in example 1 according to the present invention 2 The gas sensor is suitable for NO with different concentrations at room temperature 2 Response value change graph (fig. 6 (a)) and a curve fitting Response value (Response) to concentration (concentration) (fig. 6 (b)). According to the comparison of the test data, the response value of the sensor M1 can still reach 123% even at 2 ppm. This indicates that the prepared sensor M1 has a lower detection limit. And from the gradient fit curve, it can be seen that there is good linearity between concentration and response.
Referring to FIG. 7, FIG. 7 shows the NO produced in each of example 1 and comparative example provided in the examples of the present invention 2 A histogram of the response of the gas sensor to different types of detected gases at room temperature. SensingThe device may have various gases in the actual atmosphere detection, so ammonia (NH 3 ) Hydrogen sulfide (H) 2 S), carbon dioxide (CO) 2 ) Selectivity of Nitric Oxide (NO), acetone (acetate), formaldehyde (Formaldehyde), methanol (Methanol), xylene (Xylene) gas analysis sensor. As can be seen from fig. 7, sensor M1 is specific to NO 2 The highest response value of (2) indicates that sensor M1 is responsive to NO 2 The gas has unique selectivity.
Referring to FIG. 8, FIG. 8 is a graph showing NO produced in example 1 according to the present invention 2 Gas sensor for 100ppm NO at room temperature 2 Wherein the sensors M1 are each 100ppm NO at room temperature 2 Tested in gas. As can be seen from FIG. 8, after each response/recovery, the sensor can repeat the response/recovery process and is specific to NO 2 The response values of the sensor M1 exhibit uniformity, and the resistance of the device can return to the initial state at the end of the test, which indicates that the sensor M1 has better repeatability in the test process.
Referring to FIG. 9, FIG. 9 shows the NO produced in each of example 1 and comparative example provided in the examples of the present invention 2 Gas sensor for 100ppm NO at room temperature 2 Is a comparison of the time stability response of (c). To evaluate the time stability of the flexible gas sensor, gas sensitive performance tests were performed on sensors M1 and M0 for 14 days. As can be seen from FIG. 9, in the test for 14 days, the sensors M1 and M0 were tested at room temperature for 100ppm NO 2 The response values of (a) are respectively kept at about 290% and 335%, and the fluctuation range is kept<15, it is shown that the sensors M1 and M0 have good time stability.
Referring to FIG. 10, FIG. 10 shows the NO produced in example 1 according to the present invention 2 Gas sensor for 100ppm NO at room temperature at different tortuosity (bond) 2 A Response value (Response) change graph of (c). As can be seen from FIG. 10, the response increases and decreases with increasing curvature, and the response is 335%, 345%, 300% and the fluctuation range is less than 20% with increasing angle, because of the material during bendingWhen the material is excessively bent, the material between the electrode fingers is broken which cannot be observed by naked eyes, and the device structure is damaged, so that the response is reduced.
Referring to FIG. 11, FIG. 11 is a graph showing NO produced in example 1 according to the present invention 2 The gas sensor was cycled 500 times through bend-relaxation at room temperature at different curvatures for 100ppm NO 2 A response value variation graph of (a). As can be seen from fig. 11, the response of the sensor M1 slightly varies, and as the angle increases, the responses are 338%, 333% and 322% in order, and the fluctuation range is less than 10%, which indicates that although fine cracks appear after bending, the materials on both sides of the cracks are extruded, so that the cracks become smaller after recovery, and the thin film is kept continuous, thereby largely maintaining the sensing performance of the sensor M1.
It should be noted that in this document relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that an article or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in an article or apparatus that comprises the element. The orientation or positional relationship indicated by "upper", "lower", "left", "right", etc. is based on the orientation or positional relationship shown in the drawings, and is merely for convenience of description and to simplify the description, and is not indicative or implying that the apparatus or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as limiting the invention.
The foregoing is a further detailed description of the invention in connection with the preferred embodiments, and it is not intended that the invention be limited to the specific embodiments described. It will be apparent to those skilled in the art that several simple deductions or substitutions may be made without departing from the spirit of the invention, and these should be considered to be within the scope of the invention.
Claims (10)
1. Flexible NO 2 A method of manufacturing a gas sensor comprising:
step 1: preparing MoS by adopting a one-step hydrothermal method 2 ZnS composite;
step 2: selecting a flexible substrate, and preparing interdigital electrodes on the flexible substrate;
step 3: by using the MoS 2 Preparation of MoS on the interdigital electrode 2 ZnS composite film to obtain NO 2 A gas sensor.
2. The flexible NO according to claim 1 2 A method for manufacturing a gas sensor, wherein the step 1 includes:
step 1.1: dissolving ammonium molybdate tetrahydrate, thioacetamide and sodium dodecyl benzene sulfonate in deionized water to obtain a first mixed solution;
step 1.2: zinc acetate dihydrate is added into the first mixed solution, and the solution is stirred at room temperature until the zinc acetate dihydrate is dissolved to obtain a second mixed solution;
step 1.3: transferring the second mixed solution into a stainless steel autoclave with a Teflon lining, and placing the stainless steel autoclave with the second mixed solution into an oven for heating and reacting;
step 1.4: alternately cleaning the reacted product by using deionized water and ethanol, and drying the cleaned product in a vacuum drying oven;
step 1.5: placing the dried product in a muffle furnace, and calcining and annealing in a nitrogen environment to obtain MoS 2 ZnS composite.
3. A flexible NO according to claim 2 2 The preparation method of the gas sensor is characterized in that in the step 1.1, the mass ratio of the ammonium molybdate tetrahydrate to the thioacetamide to the sodium dodecyl benzene sulfonate is (2-4): 6:2.
4. A flexible NO according to claim 2 2 The preparation method of the gas sensor is characterized in that in the step 1.2, the mass ratio of the addition amount of zinc acetate dihydrate to the ammonium molybdate tetrahydrate in the first mixed solution is 15 (20-22).
5. A flexible NO according to claim 2 2 The preparation method of the gas sensor is characterized in that in the step 1.3, the heating temperature of an oven is 180-200 ℃ and the heating time is 12-24 hours.
6. A flexible NO according to claim 2 2 The method for manufacturing the gas sensor is characterized in that in the step 1.4, the drying temperature of the vacuum drying oven is 60 ℃ and the drying time is 12 h.
7. A flexible NO according to claim 2 2 The preparation method of the gas sensor is characterized in that in the step 1.5, the process parameters of calcination annealing are as follows: the annealing temperature is 600-800 ℃, the heating rate is 2-5 ℃/min, and the annealing time is 30-60 min.
8. The flexible NO according to claim 1 2 The preparation method of the gas sensor is characterized in that the flexible substrate comprises a PET substrate, a PDMS substrate, a PI substrate or a PEN substrate.
9. The flexible NO according to claim 1 2 The preparation method of the gas sensor is characterized in that the step 3 comprises the following steps:
by using the MoS 2 Forming MoS on the interdigital electrode by PVD, coating, spin coating or CVD process 2 ZnS composite film to obtain NO 2 A gas sensor.
10. Flexible NO 2 The gas sensor is characterized in that the gas sensor is prepared by the method of any one of claims 1-9.
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