CN110849940A - Preparation method of 3D flexible tin disulfide/graphene gas sensor for nitrogen dioxide detection - Google Patents
Preparation method of 3D flexible tin disulfide/graphene gas sensor for nitrogen dioxide detection Download PDFInfo
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- CN110849940A CN110849940A CN201911054397.1A CN201911054397A CN110849940A CN 110849940 A CN110849940 A CN 110849940A CN 201911054397 A CN201911054397 A CN 201911054397A CN 110849940 A CN110849940 A CN 110849940A
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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
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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
- G01N27/041—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body
Abstract
The invention provides 3D flexible tin disulfide/graphene (SnS) for detecting nitrogen dioxide2Method for producing an RGO) gas sensor. The method modifies SnS on the surface of graphene with a 3D structure2And SnS2the/RGO heterostructure is modified on the surface of the flexible LCP substrate to prepare the flexible gas sensor capable of detecting nitrogen dioxide in a normal temperature environment. The sensor prepared by the invention has excellent performances of high sensitivity, high selectivity and low detection limit, and the sensitivity is 6.1ppm‑1The detection limit is 8.7ppb, and the method can be applied to the field of wearable equipment.
Description
Technical Field
The invention belongs to the technical field of gas sensors, and relates to 3D flexible tin disulfide/graphene (SnS)2an/RGO) gas sensor and a method for producing the same.
Background
With the rapid development of industry and agriculture, the emission of toxic and flammable gases, such as nitrogen oxides, sulfur oxides, and carbon oxides, is a serious hazard to environmental health. Wherein nitrogen dioxide (NO)2) Can cause respiratory and cardiovascular diseases, can also cause acid rain and photochemical smog, and is considered as a typical air pollutant, the international standardNO determination2The annual safe concentration threshold of (c) is 53 ppb.
NO2And is also widely used in agriculture, medicine, military and mining. Such as synthetic manufacture of explosives and fertilizers and as biomarkers for diagnosis of lung and gastrointestinal diseases, etc., and thus, a NO having high sensitivity, high specificity, low detection limit2The gas sensor is urgently needed by the current environmental monitoring and medical diagnosis industry and is beneficial to realizing NO2High reliability and real-time monitoring.
The unique two-dimensional conjugated structure of the graphene has ultrahigh carrier mobility, and can effectively increase the carrier transmission speed and the conduction efficiency of the composite material, thereby greatly improving the response rate, shortening the response recovery time, reducing the working temperature of the sensor, and being a high-performance material for preparing the gas detection sensor.
The traditional gas sensor made of metal oxide requires high-temperature detection and oxygen environment, the gas sensor made of graphene composite material can realize detection at room temperature, energy consumption can be obviously reduced, and the graphene composite material is suitable for daily life detection requirements. The graphene can be self-assembled into a 3D porous structure composite material, and can be used for super capacitors, adsorption materials, sensors and the like. Compared with a 2D structure, the graphene with the 3D structure can provide more specific surface area and reaction sites, so that the detection sensitivity is greatly improved.
For NO2For gas-sensitive detection, a graphene-based gas-sensitive sensor has poor selectivity, which limits the practicability. Tin disulfide (SnS)2) Can be used alone as NO2Use of gas-sensitive materials for NO2The molecule has strong specific adsorption capacity, the detection limit can be lower than 1ppm, but the NO detection at room temperature can not be realized2Limit based on SnS2The gas sensor of (1) is applied in general environment. Thus modifying NO on graphene2Sensitive SnS2Can combine the performance advantages of the two, and prepare NO which has high sensitivity, high selectivity, high reliability and can be used at normal temperature2A gas sensor.
Disclosure of Invention
The object of the present invention is to solve the need for NO which is highly sensitive, highly selective, highly reliable and usable at ordinary temperatures2Problem of gas sensor, and to provide a method for NO2Detected 3D flexible tin disulfide/graphene (SnS)2Method for producing an RGO) gas sensor.
The gas sensor prepared by the invention comprises a flexible substrate and an electrode layer, wherein the surface of the flexible substrate is modified with the electrode layer, and the electrode layer comprises 3D SnS2a/RGO heterostructure layer.
The present invention uses LCP as the flexible substrate material.
The invention further aims to provide a preparation method of the 3D flexible tin disulfide/graphene gas sensor for detecting nitrogen dioxide.
The method specifically comprises the following steps:
S1、3D SnS2preparation of/RGO: under the condition of continuous stirring, adding thioacetamide and stannic chloride pentahydrate into graphene oxide solution, ultrasonically dissolving the obtained mixture, transferring the mixture into a reaction kettle for hydrothermal reaction, centrifuging and washing the obtained product to obtain solid SnS2an/RGO product;
S2、SnS2preparation of/RGO gas sensor: bonding a double-sided copper-clad LCP film on a silicon wafer by using photoresist, removing a bare copper layer on the surface of the LCP film in an etching mode, spin-coating a photoresist layer on the surface of the LCP film, sputtering a Cr/Au layer, processing an interdigital electrode on an LCP substrate by adopting a stripping technology, and processing the solid SnS prepared in the step S12and/RGO is dispersed in deionized water to prepare water dispersion, the water dispersion is deposited on the surface of the interdigital electrode of the LCP substrate, and the gas sensor is prepared after air drying.
3D SnS prepared by the invention2Detection performance and SnS of/RGO sensor2Compared with a sensor, the sensor is higher by three orders of magnitude, and SnS is modified on 3D RGO2The method greatly reduces the resistance value of the device and improves the overall detection performance of the sensor.
Further, in the step S1, the mass ratio of thioacetamide, tin chloride pentahydrate and graphene oxide is 30: 35: 4.
Further, in the step S1, the hydrothermal reaction is performed under a condition of heating at 180 ℃ for 10-12 hours.
The invention uses fine processing technology to process the interdigital electrode array on the flexible LCP substrate and leads the 3D SnS2depositing/RGO structure on the surface of base material, repeatedly bending LCP substrate, modifying electrode and SnS2the/RGO structure does not generate stripping phenomenon, and the modified SnS is shown2the/RGO structure has strong adhesion, and the sensor can be used for wearable equipment and flexible devices.
Further, in the step S2, the silicon wafer has a thickness of 300 μm.
Further, in step S2, the spin-on photoresist has a thickness of 5 μm.
Further, in step S2, the thickness of the sputtered Cr layer is 8nm, and the thickness of the Au layer is 280 nm.
Further, in the step S2, the concentration of the aqueous dispersion is 2.0 mg/mL.
The 3D SnS prepared by the method is subjected to SEM, Raman spectrum, XPS and the like2the/RGO is characterized.
As shown in attached figure 2, 3D SnS prepared by the invention2SEM picture of/RGO. As can be seen in the figure, SnS prepared by the invention2the/RGO structure has a porous structure, the size of the pores ranges from hundreds of nanometers to several micrometers, and NO is facilitated2Diffusion and adsorption of molecules. After the hydrothermal reaction, the hydrophilic graphene oxide is deoxidized to graphene and restores a conjugated structure due to its hydrophobic interaction and
the interaction forms a 3D porous structure.
As shown in attached figure 3, 3D SnS prepared by the invention2Raman spectrum of/RGO. As can be seen in the figure, SnS2Two typical peaks appear on Raman spectra of/RGO and GO (graphene oxide), and are respectively located at 1354cm-1D band and 1590cm-1The G band, the D band and the G band correspond to the disorder and the first-order scattering of the graphene 2D mode respectively, ID：IGFrom 0.90 liter of GO to SnS21.17 of/RGO, which shows that the defect sites on the surface of the graphene can be used as NO when the defect sites on the graphene are increased after the hydrothermal reaction2Is available to the active adsorption sites of (1), contributes NO2Sensitivity of detection is improved, and in SnS2The Raman spectrum of the/RGO is observed to be at 311cm-1The peak is not observed on a GO spectrogram, and the SnS on the surface of the graphene is verified2Is performed.
As shown in attached figure 4, 3D SnS prepared by the invention2XPS profile of/RGO. As can be seen in the figure, SnS2The composition of/RGO was high C (75.18% at%), small amounts of O (16.15% at%), Sn (2.48% at%) and S (6.19% at%), while that of GO was C (65.5% at%) and O (34.5% at%).
For the 3D SnS prepared by the invention2NO with/RGO gas sensor2And testing the gas detection performance.
As shown in FIG. 5, SnS prepared for the invention of example 12/RGO and conventional SnS2And an RGO (graphene) gas sensor for 0.5-8 ppm NO at normal temperature2Response curve of gas. As can be seen in the figure, SnS2Response data of/RGO sensor and RGO sensor with NO2Increase in gas concentration, SnS2/RGO sensor and RGO sensor for 8ppm NO2The change in the gas response rates were 49.5% and 2.2%, respectively, and it can be concluded that SnS was modified on RGO2Then, SnS prepared by the invention2/RGO gas sensor for NO2The response performance of the gas is 22.6 times that of the graphene sensor.
As shown in FIG. 6, SnS prepared for the invention of example 12the/RGO gas sensor can measure 0-400 ppb NO at normal temperature2Response curve of gas. This shows that the SnS prepared by the invention2the/RGO gas sensor has the function of detecting NO with extremely low concentration2Gas capability, which graphene gas sensors do not have.
As shown in FIG. 7, SnS prepared for the invention of example 12/RGO gas sensor and traditional SnS2And the RGO gas sensor is used for detecting 0-8 ppm NO at normal temperature2Linear fit curve for gas continuous test. This shows that the SnS prepared by the invention2the/RGO gas sensor possesses the same NO2The response performance of the gas can be calculated to obtain SnS2Sensitivity of the/RGO gas sensor is 6.1ppm-1The detection limit is 8.7ppb, which is several orders of magnitude lower than that of graphene sensors, and the graphene sensor has the characteristics of high sensitivity and low detection limit.
As shown in FIG. 8, SnS prepared for the invention of example 12RGO gas sensor for 2ppm NO2And (5) testing the repeatability of the gas. It can be seen that after repeating three test cycles, the response rate change is substantially consistent and is 14.3%, and the sensor response signal can be rapidly recovered in a short time, which indicates that the SnS prepared by the invention2the/RGO gas sensor has good repeatability and reversibility.
As shown in FIG. 9, SnS prepared for the invention of example 12Bending test of the/RGO gas sensor. As can be seen in the figure, the response rate of the flexible sensor is basically not changed after the flexible sensor is bent by 120 degrees, which shows that the SnS prepared by the invention has no change under the condition of mechanical deformation2The detection performance of the/RGO gas sensor is not affected, and the method can be applied to the fields of wearable equipment, electronic skin and the like.
As shown in FIG. 10, SnS prepared for the invention of example 12Anti-interference test of/RGO gas sensor. It can be seen that for common interfering gaseous species, e.g. 50ppm NH3、1000ppm CO2Saturated VOC vapor, etc., sensor pair 8ppm NO2The gas response is more than 15 times higher than that of the interference gas, which shows that the SnS prepared by the invention2the/RGO gas sensor has good selectivity and anti-interference performance.
The method modifies SnS on the surface of graphene with a 3D structure2Is NO2Gas molecules provide additional active sites and charge transfer paths while SnS2The nano/micron pores on the 3D structure of/RGO are also NO2Gas molecules provide more charge transfer paths, whereas SnS2By forming a hetero-phase with RGOStructure promoting electron transfer from RGO to NO2Gas molecules are transferred, so that energy consumption is reduced, and sensitivity is improved.
The invention prepares 3D SnS on a flexible LCP substrate2the/RGO heterostructure can keep high sensitivity and high reliability under the condition of high bending and can realize NO treatment under the normal temperature condition2High sensitivity and high selectivity detection.
The invention has the beneficial effects that:
(1) the invention provides a flexible and feasible low-cost 3D SnS2The preparation method of the/RGO gas sensor has the advantages of high sensitivity, high selectivity and low detection limit.
(2) SnS prepared by the invention2the/RGO gas sensor can carry out NO at normal temperature2Detection of gas avoids conventional NO2The gas sensor needs high temperature detection environment, can be used for daily life, and has wider application range.
(3) SnS prepared by the invention2the/RGO gas sensor adopts a flexible base material, can be bent, does not influence the detection performance, and can be applied to new fields such as wearable equipment and electronic skin.
Drawings
The invention is further illustrated by means of the attached drawings, but the embodiments in the drawings do not constitute any limitation to the invention, and for a person skilled in the art, other drawings can be obtained on the basis of the following drawings without inventive effort.
FIG. 1 shows SnS prepared by the present invention2A real object diagram of the/RGO gas sensor;
FIG. 2 shows SnS prepared by the present invention2SEM picture of/RGO;
FIG. 3 shows SnS prepared by the present invention2Raman spectrum of/RGO;
FIG. 4 shows SnS prepared by the present invention2XPS profile of/RGO;
FIG. 5 shows SnS prepared in example 1 of the present invention2/RGO and SnS2And the RGO gas sensor is used for detecting 0.5-8 ppm NO at normal temperature2The response curve of the gas;
FIG. 6 shows SnS prepared in example 1 of the present invention2the/RGO gas sensor can measure 50-400 ppb NO at normal temperature2The response curve of the gas;
FIG. 7 shows SnS prepared in example 1 of the present invention2/RGO gas sensor and SnS2And the RGO gas sensor is used for detecting 0-8 ppm NO at normal temperature2A linear fit curve for gas continuous testing;
FIG. 8 shows SnS prepared in example 1 of the present invention2RGO gas sensor for 2ppm NO2Testing the repeatability of the gas;
FIG. 9 shows SnS prepared in example 1 of the present invention2Bending test of the/RGO gas sensor;
FIG. 10 shows SnS prepared in example 1 of the present invention2Anti-interference test of/RGO gas sensor.
Detailed Description
In order that the objects, aspects and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the following detailed description and the accompanying drawings.
Example 1
3D Flexible SnS2Preparation of/RGO gas sensor:
(1)3D SnS2preparation of/RGO
Under the condition of continuous stirring, 0.30g of thioacetamide and 0.35g of stannic chloride pentahydrate are added into 20mL of graphene oxide solution with the concentration of 0.2mg/mL, the obtained mixture is ultrasonically dissolved and then transferred into a reaction kettle to be heated for 11h at the temperature of 180 ℃, the obtained product is centrifugally treated and washed by deionized water to obtain solid SnS2the/RGO product.
(2)SnS2Preparation of/RGO gas sensor
Bonding an LCP film with copper coated on both sides on a silicon wafer with the thickness of 300 mu m by using photoresist, removing a copper layer exposed on the surface of the LCP film in an etching mode, spin-coating a photoresist layer with the thickness of 5 mu m on the surface of the LCP film, sputtering an 8nm Cr/280nm Au layer, processing an interdigital electrode on an LCP substrate by adopting a stripping technology, and carrying out solid SnS treatment on the LCP substrate prepared in the step S12/RGO redispersion inAnd preparing aqueous dispersion with the concentration of 2.0mg/mL in the ionized water, depositing the aqueous dispersion on the surface of the interdigital electrode of the LCP substrate, and air-drying to obtain the gas sensor.
Prepared SnS2A physical diagram of the/RGO gas sensor is shown in FIG. 1.
Example 2
3D Flexible SnS2Preparation of/RGO gas sensor:
(1)3D SnS2preparation of/RGO
Under the condition of continuous stirring, 0.60g of thioacetamide and 0.70g of stannic chloride pentahydrate are added into 40mL of graphene oxide solution with the concentration of 0.2mg/mL, the obtained mixture is ultrasonically dissolved and then transferred into a reaction kettle to be heated for 10 hours at the temperature of 180 ℃, the obtained product is centrifugally treated and washed by deionized water to obtain solid SnS2the/RGO product.
(2)SnS2Preparation of/RGO gas sensor
Bonding an LCP film with copper coated on both sides on a silicon wafer with the thickness of 300 mu m by using photoresist, removing a copper layer exposed on the surface of the LCP film in an etching mode, spin-coating a photoresist layer with the thickness of 5 mu m on the surface of the LCP film, sputtering an 8nm Cr/280nm Au layer, processing an interdigital electrode on an LCP substrate by adopting a stripping technology, and carrying out solid SnS treatment on the LCP substrate prepared in the step S12the/RGO is re-dispersed in deionized water to prepare aqueous dispersion with the concentration of 2.0mg/mL, and the aqueous dispersion is deposited on the surface of the interdigital electrode of the LCP substrate and air-dried to prepare the gas sensor.
Example 3
3D Flexible SnS2Preparation of/RGO gas sensor:
(1)3D SnS2preparation of/RGO
Under the condition of continuous stirring, 0.90g of thioacetamide and 1.05g of stannic chloride pentahydrate are added into 60mL of graphene oxide solution with the concentration of 0.2mg/mL, the obtained mixture is transferred into a reaction kettle after being dissolved by ultrasound, the reaction kettle is heated for 12 hours at the temperature of 180 ℃, the obtained product is centrifuged and washed by deionized water, and solid SnS is obtained2the/RGO product.
(2)SnS2Preparation of/RGO gas sensor
Bonding an LCP film with copper coated on both sides on a silicon wafer with the thickness of 300 mu m by using photoresist, removing a copper layer exposed on the surface of the LCP film in an etching mode, spin-coating a photoresist layer with the thickness of 5 mu m on the surface of the LCP film, sputtering an 8nm Cr/280nm Au layer, processing an interdigital electrode on an LCP substrate by adopting a stripping technology, and carrying out solid SnS treatment on the LCP substrate prepared in the step S12the/RGO is re-dispersed in deionized water to prepare aqueous dispersion with the concentration of 2.0mg/mL, and the aqueous dispersion is deposited on the surface of the interdigital electrode of the LCP substrate and air-dried to prepare the gas sensor.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single technical solution, and such description is for clarity only, and those skilled in the art should take the description as a whole, and the technical solutions in the embodiments may be combined appropriately to form other embodiments that those skilled in the art can understand. The technical details not described in detail in the present invention can be implemented by any of the prior arts in the field. In particular, all technical features of the invention which are not described in detail can be achieved by any prior art.
Claims (9)
1. A3D flexible tin disulfide/graphene gas sensor for nitrogen dioxide detection is characterized by comprising a flexible substrate and an electrode layer, wherein the flexible substrate is modified on the surface of the electrode layer, and the electrode layer comprises 3D SnS2a/RGO heterostructure layer.
2. The 3D flexible tin disulfide/graphene gas sensor for nitrogen dioxide detection as claimed in claim 1, wherein said flexible substrate material is LCP.
3. The preparation method of the 3D flexible tin disulfide/graphene gas sensor for nitrogen dioxide detection according to claim 1, comprising the following steps:
S1、3D SnS2preparation of/RGO: under the condition of continuous stirring, adding thioacetamide and stannic chloride pentahydrate into graphene oxide solution, ultrasonically dissolving the obtained mixture, transferring the mixture into a reaction kettle for hydrothermal reaction, centrifuging and washing the obtained product to obtain solid SnS2an/RGO product;
S2、SnS2preparation of/RGO gas sensor: bonding a double-sided copper-clad LCP film on a silicon wafer by using photoresist, removing a bare copper layer on the surface of the LCP film in an etching mode, spin-coating a photoresist layer on the surface of the LCP film, sputtering a Cr/Au layer, processing an interdigital electrode on an LCP substrate by adopting a stripping technology, and processing the solid SnS prepared in the step S12and/RGO is dispersed in deionized water to prepare water dispersion, the water dispersion is deposited on the surface of the interdigital electrode of the LCP substrate, and the gas sensor is prepared after air drying.
4. The method for preparing the 3D flexible tin disulfide/graphene gas sensor for detecting nitrogen dioxide, prepared according to the method of claim 3, wherein in the step S1, the mass ratio of thioacetamide, tin chloride pentahydrate and graphene oxide is 30: 35: 4.
5. The method for preparing the 3D flexible tin disulfide/graphene gas sensor for nitrogen dioxide detection according to the method of claim 3, wherein in the step S1, the hydrothermal reaction condition is heating at 180 ℃ for 10-12 h.
6. The method for preparing the 3D flexible tin disulfide/graphene gas sensor for detecting nitrogen dioxide, which is prepared according to the method of claim 3, wherein in the step S2, the thickness of the silicon wafer is 300 μm.
7. The method for preparing a 3D flexible tin disulfide/graphene gas sensor for nitrogen dioxide detection according to claim 3, wherein in step S2, the spin-on photoresist has a thickness of 5 μm.
8. The method for preparing the 3D flexible tin disulfide/graphene gas sensor for detecting nitrogen dioxide, which is prepared according to the method of claim 3, wherein in the step S2, the thickness of the sputtered Cr layer is 8nm, and the thickness of the Au layer is 280 nm.
9. The method for preparing a 3D flexible tin disulfide/graphene gas sensor for nitrogen dioxide detection according to the method of claim 3, wherein in the step S2, the concentration of the aqueous dispersion is 2.0 mg/mL.
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