CN109342522B - Polypyrrole/graphene composite material-based resistance type NH3Sensor, preparation method and application thereof - Google Patents
Polypyrrole/graphene composite material-based resistance type NH3Sensor, preparation method and application thereof Download PDFInfo
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Abstract
Polypyrrole/graphene composite material-based resistance type NH3A sensor, a preparation method and an application thereof belong to the technical field of gas sensors. Using ceramic plate as substrate, adopting screen printing technique to deposit carbon interdigital electrode on the surface of ceramic plate,the carbon interdigital electrode is connected with a lead, the surfaces of the ceramic chip and the carbon interdigital electrode are coated with a gas sensitive film, the gas sensitive film is a polypyrrole/graphene composite material, and the thickness of the film is 10-30 micrometers; the resistance of the gas sensitive film can change before and after the gas sensitive film contacts the gas to be measured, and the sensitivity of the sensor can be obtained by measuring the change of the resistance between the carbon interdigital electrodes. The composite material solution prepared by the invention can be used for forming a film on the interdigital electrode by methods such as spin coating and the like, is easy to process, can be used for conveniently preparing the gas sensor, and solves the problems that the traditional metal oxide gas sensor needs high-temperature sintering and is complex to process.
Description
Technical Field
The invention belongs to the technical field of gas sensors, particularly relates to a graphene-based resistance type gas sensor with room-temperature gas-sensitive response characteristic, a preparation method and application thereof, and particularly relates to a polypyrrole/graphene composite material-based resistance type NH3A sensor, a preparation method and application thereof.
Background
Ammonia gas (NH)3) The liquid ammonia refrigerating fluid is a typical toxic and harmful gas, mainly comes from industrial production of chemical fertilizers and the like, volatilization of liquid ammonia refrigerating fluid, the field of organic chemical industry, release of indoor decoration materials and the like, and brings serious harm to human health. For NH in atmospheric environment3The accurate measurement and continuous detection are carried out to treat NH3The primary condition of pollution is one of the research hotspots in the field of environmental protection at present. Although a chemical analysis instrument typified by gas chromatography can accurately measure NH in the atmospheric environment3However, the application of the instrument in various research fields is limited by the defects of large volume, high cost, requirement of professional operation and the like, and particularly, the construction of the internet of things shows obvious defects. The gas sensor is an important chemical sensor and has wide application in the fields of industrial and agricultural production, process control, environmental monitoring and protection, anti-terrorism and the like. Development of high-performance NH with the advantages of high sensitivity, low cost, low power consumption, miniaturization and the like3Sensors have become a research hotspot in the scientific research field and the industrial field.
At present, semiconductor oxides represented by tin dioxide and zinc oxide become the most widely used sensitive materials, and have the advantages of convenience in preparation, low cost, wide sources and the like. Metal oxides in the pure state are generally difficult to express as NH3Good sensitivity performance. Although the modified metal oxide can realize the reaction to NH3Good sensitivity, but these devices also have some disadvantages, such as poor stability, high influence from humidity, less than ideal selectivity, etc. In particular, metal oxide based gas sensors need to operate at relatively high temperatures (typically above 200 ℃), which makes the power consumption of the components large, makes it difficult to prepare portable instruments, and limits their applications.
In order to solve this problem, the operating temperature of the sensor is lowered, and the development of a gas sensitive material operating at room temperature is receiving wide attention from researchers. The conductive polymer material represented by polyaniline and polypyrrole can realize room temperature NH detection3However, the response characteristic is poor, and the device is greatly influenced by environmental conditions such as temperature and humidity. In recent years, two-dimensional carbon-based nanomaterials represented by graphene have been developed rapidly, and become a hot spot of research in the material field. Graphene has room temperature conductivity and fast carrier mobility for developing room temperature operating NH3Gas sensitive materials provide a new concept. Researches find that the graphene material can really realize room temperature detection of NH3However, the sensitivity of the manufactured sensor is low, and the response recovery rate is slow. Recently, conducting polymers are adopted to carry out surface modification on graphene, the synergistic effect of the conducting polymers and the graphene is fully exerted, and high-sensitivity NH detection at room temperature is hopefully realized3. The development of graphene-based room temperature gas sensors is one of the important directions for the research of the sensor field, and the development is very rapid.
Disclosure of Invention
It is an object of the present invention to provide a method for producing NH with high sensitivity at room temperature3Polypyrrole/graphene composite material-based resistance type NH with response characteristic3Sensor, preparation method and application thereofThe application is as follows.
The invention relates to a resistance type NH based on a polypyrrole/graphene composite material3The sensor is characterized in that a ceramic wafer is used as a substrate, carbon interdigital electrodes are deposited on the surface of the ceramic wafer by adopting a screen printing technology, the thickness of the electrodes is 1-2 mu m, the number of pairs of the electrodes is 4-6, and the width of each electrode is 50-100 mu m; the carbon interdigital electrode is connected with a lead, the surfaces of the ceramic chip and the carbon interdigital electrode are coated with a gas sensitive film, the gas sensitive film is a polypyrrole/graphene composite material, and the thickness of the film is 10-30 micrometers; the resistance of the gas sensitive film changes before and after the gas sensitive film contacts the gas to be measured, a 5V voltage is applied to two ends of the carbon electrode by using an intelligent gas sensitive analysis system (CGS-8, Beijing Elite technology, Inc.), the sensitivity of the sensor can be obtained by measuring the change of the resistance between the carbon interdigital electrodes, and the calculation method of the sensitivity is that the resistance value of the carbon electrode in ammonia gas is divided by the resistance value of the carbon electrode in air.
The polypyrrole/graphene composite material is prepared by mixing (surface loading) graphene and polypyrrole, wherein the mass ratio of the graphene to the polypyrrole is 1:3 to 80.8.
The invention relates to a resistance type NH based on a polypyrrole/graphene composite material3The preparation method of the sensor comprises the following steps:
(1) taking a ceramic wafer as a substrate, depositing carbon interdigital electrodes on the surface of the ceramic wafer by adopting a screen printing technology, wherein the thickness of the electrodes is 1-2 mu m, the number of pairs of the electrodes is 4-6, and the width of each electrode is 50-100 mu m;
(2) ultrasonically cleaning a ceramic wafer substrate with carbon interdigital electrodes on the surface by using ethanol and water in sequence, and drying;
(3) preparing 30-40 mL of graphene oxide aqueous solution, wherein the concentration of the graphene oxide is 0.1-5 mg/mL;
(4) and (3) adding 0.1-1.0 mL of pyrrole into the graphene oxide aqueous solution prepared in the step (3), stirring for 24-36 hours at room temperature, performing centrifugal separation on the obtained composite material solution, washing with water, and drying to obtain a pyrrole/graphene oxide composite material, wherein the mass ratio of graphene oxide to pyrrole is 1:2.4 to 64.6;
(5) adding the pyrrole/graphene oxide composite material prepared in the step (4) into water with the volume of 30-40 mL, performing ultrasonic dispersion to fully mix the materials, performing hydrothermal reaction on the solution at 160-180 ℃ for 12-24 hours to obtain a polypyrrole/graphene composite material solution, performing centrifugal separation on the composite material solution, washing with water, and drying to obtain the polypyrrole/graphene composite material, wherein the mass ratio of graphene to polypyrrole is 1:3 to 80.8;
(6) dispersing the polypyrrole/graphene composite material prepared in the step (5) into water, wherein the concentration of a composite material water solution is 1-10 mg/mL; and (3) the solution is coated on the surface of the ceramic wafer substrate with the carbon interdigital electrode obtained in the step (2) in a suspension manner, and then heat treatment is carried out for 1-4 hours at the temperature of 80-130 ℃, so that the thickness of the obtained sensitive film is 10-30 mu m, and the polypyrrole/graphene composite material-based resistance type gas sensor is prepared.
The gas sensor prepared by the invention is used for NH3Room temperature response of (1), NH3The detection concentration of (2) is 10ppm to 100ppm, the lowest detectable concentration is 10ppm, and the sensitivity is 9.36%.
The invention has the advantages that:
1) the interdigital electrode is prepared by adopting a screen printing technology, so that the cost is low, the structure is easy to regulate and control, and the product consistency is high; the strong pi-pi action between the carbon electrode and the graphene material can improve the adhesion between the sensitive film and the electrode and improve the stability of the device.
2) The polypyrrole/graphene composite material is prepared by a hydrothermal method, and the method is simple, easy to operate and low in cost. And the regulation and control of the properties of the graphene-based composite material such as the composition, the structure and the like can be realized by controlling experimental parameters such as the reaction temperature, the reaction time, the proportion of the reaction precursor and the like.
3) The introduction of polypyrrole into the composite material can further prevent the agglomeration of graphene sheet layers, and effectively improve the specific surface area of the composite material.
4) The introduction of the graphene in the composite material can obviously improve the conductivity of the sensitive material.
5) Polypyrrole is modified on the surface of graphene in the composite material, and the surface active site is regulated and controlled to improve the sensitivity of the sensor by virtue of the surface active site of the polypyrrole.
6) The prepared composite material solution can be formed into a film on the interdigital electrode by methods such as spin coating and the like, is easy to process, can be used for conveniently preparing the gas sensor, and solves the problems that the traditional metal oxide gas sensor needs high-temperature sintering and is complex to process.
Drawings
Fig. 1 is a schematic structural view of a gas sensor according to the present invention.
Wherein: ceramic wafer substrate 1, carbon interdigital electrodes 2 and 3, gas sensitive film 4, and leads 5 and 6.
Fig. 2 is a scanning electron micrograph of the polypyrrole/graphene composite material.
FIG. 3 shows a polypyrrole/graphene composite gas sensor for 10 ppm-100 ppm NH3Room temperature dynamic response recovery curve.
FIG. 4 is a polypyrrole/graphene composite gas sensor vs. 100ppm NH3Continuous cycle test curve of (2).
Detailed Description
The invention is further illustrated below with reference to the figures and examples.
Example 1
(1) Taking a ceramic wafer as a substrate, depositing carbon interdigital electrodes on the surface of the ceramic wafer by adopting a screen printing technology, wherein the thickness of the electrodes is 2 mu m, the number of pairs of the electrodes is 4, and the width of each electrode is 50 mu m;
(2) ultrasonically cleaning a ceramic wafer substrate with carbon interdigital electrodes on the surface by using ethanol and water in sequence, and drying;
(3) preparing a graphene oxide aqueous solution, wherein the concentration of the graphene oxide aqueous solution is 0.1mg/mL, and the volume of the graphene oxide aqueous solution is 30 mL;
(4) and (3) then adding 0.1mL of pyrrole into the graphene oxide solution prepared in the step (3), stirring for 24 hours at room temperature, centrifugally separating, washing and drying the composite material solution to obtain a pyrrole/graphene oxide composite material, wherein the mass ratio of graphene oxide to pyrrole is 1: 32.3;
(5) adding the pyrrole/graphene oxide composite material prepared in the step (4) into water with the volume of 30mL, performing ultrasonic dispersion to fully mix the pyrrole/graphene oxide composite material and the water, performing hydrothermal reaction on the solution at 160 ℃ for 24 hours to obtain a polypyrrole/graphene composite material solution, performing centrifugal separation, water washing and drying on the composite material solution to obtain the polypyrrole/graphene composite material, wherein the mass ratio of graphene to polypyrrole is 1: 40.4;
(6) dispersing the polypyrrole/graphene composite material prepared in the step (5) into water, wherein the concentration of the composite material aqueous solution is 1 mg/mL; and (3) the solution is coated on the surface of the ceramic wafer substrate with the carbon interdigital electrode obtained in the step (2) in a suspension manner, and then the ceramic wafer substrate is subjected to heat treatment at 80 ℃ for 1 hour to obtain a sensitive film with the thickness of 10 mu m, so that the polypyrrole/graphene composite material-based resistance type gas sensor is prepared.
Example 2
(1) Taking a ceramic wafer as a substrate, depositing carbon interdigital electrodes on the surface of the ceramic wafer by adopting a screen printing technology, wherein the thickness of the electrodes is 2 mu m, the number of pairs of the electrodes is 5, and the width of each electrode is 80 mu m;
(2) ultrasonically cleaning a ceramic wafer substrate with carbon interdigital electrodes on the surface by using ethanol and water in sequence, and drying;
(3) preparing a graphene oxide aqueous solution, wherein the concentration of the graphene oxide aqueous solution is 0.25mg/mL, and the volume of the graphene oxide aqueous solution is 40 mL;
(4) and (3) then adding 0.5mL of pyrrole into the graphene oxide solution prepared in the step (3), stirring for 30 hours at room temperature, centrifugally separating, washing and drying the composite material solution to obtain a pyrrole/graphene oxide composite material, wherein the mass ratio of graphene oxide to pyrrole is 1: 48.5;
(5) adding the pyrrole/graphene oxide composite material prepared in the step (4) into water with the volume of 40mL, performing ultrasonic dispersion to fully mix the pyrrole/graphene oxide composite material, performing hydrothermal reaction on the solution at 160 ℃ for 12 hours to obtain a polypyrrole/graphene composite material solution, performing centrifugal separation, water washing and drying on the composite material solution to obtain the polypyrrole/graphene composite material, wherein the mass ratio of graphene to polypyrrole is 1: 60.6 of the total weight of the mixture;
(6) dispersing the polypyrrole/graphene composite material prepared in the step (5) into water, wherein the concentration of the composite material aqueous solution is 2.5 mg/mL; and (3) the solution is coated on the surface of the ceramic wafer substrate with the carbon interdigital electrode obtained in the step (2) in a suspension manner, and then the ceramic wafer substrate is subjected to heat treatment at 90 ℃ for 2 hours to obtain a sensitive film with the thickness of 20 microns, so that the polypyrrole/graphene composite material-based resistance type gas sensor is prepared.
Example 3
(1) Taking a ceramic wafer as a substrate, depositing carbon interdigital electrodes on the surface of the ceramic wafer by adopting a screen printing technology, wherein the thickness of the electrodes is 2 mu m, the number of pairs of the electrodes is 6, and the width of each electrode is 100 mu m;
(2) ultrasonically cleaning a ceramic wafer substrate with carbon interdigital electrodes on the surface by using ethanol and water in sequence, and drying;
(3) preparing a graphene oxide aqueous solution, wherein the concentration of the graphene oxide aqueous solution is 0.5mg/mL, and the volume of the graphene oxide aqueous solution is 30 mL;
(4) then adding 1.0mL of pyrrole into the graphene oxide solution prepared in the step (3), stirring for 36 hours at room temperature, carrying out centrifugal separation, washing and drying on the composite material solution to obtain a pyrrole/graphene oxide composite material, wherein the mass ratio of the graphene oxide to the pyrrole is 1: 64.6;
(5) adding the pyrrole/graphene oxide composite material prepared in the step (4) into 30mL of water, performing ultrasonic dispersion to fully mix the pyrrole/graphene oxide composite material and the water, performing hydrothermal reaction on the solution at 170 ℃ for 24 hours to obtain a polypyrrole/graphene composite material solution, performing centrifugal separation on the composite material solution, washing with water, and drying to obtain a polypyrrole/graphene composite material, wherein the mass ratio of graphene to polypyrrole is 1: 80.8;
(6) dispersing the polypyrrole/graphene composite material prepared in the step (5) into water, wherein the concentration of the composite material aqueous solution is 5 mg/mL; and (3) the solution is coated on the surface of the ceramic wafer substrate with the carbon interdigital electrode obtained in the step (2) in a suspension manner, and then the ceramic wafer substrate is subjected to heat treatment at 100 ℃ for 3 hours to obtain a sensitive film with the thickness of 30 microns, so that the polypyrrole/graphene composite material-based resistance type gas sensor is prepared.
Example 4
(1) Taking a ceramic wafer as a substrate, depositing carbon interdigital electrodes on the surface of the ceramic wafer by adopting a screen printing technology, wherein the thickness of the electrodes is 1 mu m, the number of pairs of the electrodes is 4, and the width of each electrode is 50 mu m;
(2) ultrasonically cleaning a ceramic wafer substrate with carbon interdigital electrodes on the surface by using ethanol and water in sequence, and drying;
(3) preparing a graphene oxide aqueous solution, wherein the concentration of the graphene oxide aqueous solution is 1mg/mL, and the volume of the graphene oxide aqueous solution is 40 mL;
(4) then adding 0.1mL of pyrrole into the graphene oxide solution prepared in the step (3), stirring for 24 hours at room temperature, carrying out centrifugal separation, washing and drying on the composite material solution to obtain a pyrrole/graphene oxide composite material, wherein the mass ratio of the graphene oxide to the pyrrole is 1: 2.4;
(5) adding the pyrrole/graphene oxide composite material prepared in the step (4) into water with the volume of 40mL, performing ultrasonic dispersion to fully mix the pyrrole/graphene oxide composite material, performing hydrothermal reaction on the solution at 170 ℃ for 12 hours to obtain a polypyrrole/graphene composite material solution, performing centrifugal separation on the composite material solution, washing with water, and drying to obtain a polypyrrole/graphene composite material, wherein the mass ratio of graphene to polypyrrole is 1: 3;
(6) dispersing the polypyrrole/graphene composite material prepared in the step (5) into water, wherein the concentration of the composite material aqueous solution is 7.5 mg/mL; and (3) the solution is coated on the surface of the ceramic wafer substrate with the carbon interdigital electrode obtained in the step (2) in a suspension manner, and then the ceramic wafer substrate is subjected to heat treatment at 110 ℃ for 3 hours to obtain a sensitive film with the thickness of 10 microns, so that the polypyrrole/graphene composite material-based resistance type gas sensor is prepared.
Example 5
(1) Taking a ceramic wafer as a substrate, depositing carbon interdigital electrodes on the surface of the ceramic wafer by adopting a screen printing technology, wherein the thickness of the electrodes is 1 mu m, the number of pairs of the electrodes is 5, and the width of each electrode is 80 mu m;
(2) ultrasonically cleaning a ceramic wafer substrate with carbon interdigital electrodes on the surface by using ethanol and water in sequence, and drying;
(3) preparing a graphene oxide aqueous solution, wherein the concentration of the graphene oxide aqueous solution is 2.5mg/mL, and the volume of the graphene oxide aqueous solution is 30 mL;
(4) then adding 0.5mL of pyrrole into the graphene oxide solution prepared in the step (3), stirring for 30 hours at room temperature, carrying out centrifugal separation, washing and drying on the composite material solution to obtain a pyrrole/graphene oxide composite material, wherein the mass ratio of the graphene oxide to the pyrrole is 1: 6.5;
(5) adding the pyrrole/graphene oxide composite material prepared in the step (4) into 30mL of water, performing ultrasonic dispersion to fully mix the pyrrole/graphene oxide composite material and the water, performing hydrothermal reaction on the solution at 180 ℃ for 24 hours to obtain a polypyrrole/graphene composite material solution, performing centrifugal separation on the composite material solution, washing with water, and drying to obtain a polypyrrole/graphene composite material, wherein the mass ratio of graphene to polypyrrole is 1: 8.1;
(6) dispersing the polypyrrole/graphene composite material prepared in the step (5) into water, wherein the concentration of the composite material aqueous solution is 10 mg/mL; and (3) the solution is coated on the surface of the ceramic wafer substrate with the carbon interdigital electrode obtained in the step (2) in a suspension manner, and then the ceramic wafer substrate is subjected to heat treatment at 120 ℃ for 4 hours to obtain a sensitive film with the thickness of 20 microns, so that the polypyrrole/graphene composite material-based resistance type gas sensor is prepared.
Example 6
(1) Taking a ceramic wafer as a substrate, depositing carbon interdigital electrodes on the surface of the ceramic wafer by adopting a screen printing technology, wherein the thickness of the electrodes is 1 mu m, the number of pairs of the electrodes is 6, and the width of each electrode is 100 mu m;
(2) ultrasonically cleaning a ceramic wafer substrate with carbon interdigital electrodes on the surface by using ethanol and water in sequence, and drying;
(3) preparing a graphene oxide aqueous solution, wherein the concentration of the graphene oxide aqueous solution is 5mg/mL, and the volume of the graphene oxide aqueous solution is 40 mL;
(4) then adding 1.0mL of pyrrole into the graphene oxide solution prepared in the step (3), stirring for 36 hours at room temperature, carrying out centrifugal separation, washing and drying on the composite material solution to obtain a pyrrole/graphene oxide composite material, wherein the mass ratio of the graphene oxide to the pyrrole is 1: 4.85;
(5) adding the pyrrole/graphene oxide composite material prepared in the step (4) into water with the volume of 40mL, performing ultrasonic dispersion to fully mix the pyrrole/graphene oxide composite material, performing hydrothermal reaction on the solution at 180 ℃ for 12 hours to obtain a polypyrrole/graphene composite material solution, performing centrifugal separation on the composite material solution, washing with water, and drying to obtain a polypyrrole/graphene composite material, wherein the mass ratio of graphene to polypyrrole is 1: 6;
(6) dispersing the polypyrrole/graphene composite material prepared in the step (5) into water, wherein the concentration of the composite material aqueous solution is 10 mg/mL; and (3) the solution is coated on the surface of the ceramic wafer substrate with the carbon interdigital electrode obtained in the step (2) in a suspension manner, and then the ceramic wafer substrate is subjected to heat treatment at 130 ℃ for 4 hours to obtain a sensitive film with the thickness of 30 microns, so that the polypyrrole/graphene composite material-based resistance type gas sensor is prepared.
A scanning electron micrograph of the polypyrrole/graphene composite material prepared in example 1 is shown in fig. 2, and as can be seen from fig. 2, the composite material has a typical lamellar structure similar to graphene, and a large amount of polypyrrole nanoparticles are distributed on the surface of the graphene lamellae.
The response recovery curves of the polypyrrole/graphene composite gas sensor prepared in example 1 at room temperature for different concentrations of ammonia gas are shown in fig. 3. It can be seen that the prepared graphene-based gas sensor has high and quick response to ammonia gas with different concentrations, and the response time is less than 1 minute.
The cycle stability test curve of the polypyrrole/graphene composite gas sensor prepared in example 1 at room temperature against 100ppm ammonia gas is shown in fig. 4. It can be seen that the sensor is paired with NH3Showing good cycling stability.
Claims (3)
1. Polypyrrole/graphene composite material-based resistance type NH3The preparation method of the sensor comprises the following steps:
(1) taking a ceramic wafer as a substrate, depositing carbon interdigital electrodes on the surface of the ceramic wafer by adopting a screen printing technology, wherein the thickness of the electrodes is 1-2 mu m, the number of pairs of the electrodes is 4-6, and the width of each electrode is 50-100 mu m;
(2) ultrasonically cleaning a ceramic wafer substrate with carbon interdigital electrodes on the surface by using ethanol and water in sequence, and drying;
(3) preparing 30-40 mL of graphene oxide aqueous solution, wherein the concentration of the graphene oxide is 0.1-5 mg/mL;
(4) and (3) adding 0.1-1.0 mL of pyrrole into the graphene oxide aqueous solution prepared in the step (3), stirring for 24-36 hours at room temperature, performing centrifugal separation on the obtained composite material solution, washing with water, and drying to obtain a pyrrole/graphene oxide composite material, wherein the mass ratio of graphene oxide to pyrrole is 1:2.4 to 64.6;
(5) adding the pyrrole/graphene oxide composite material prepared in the step (4) into water with the volume of 30-40 mL, performing ultrasonic dispersion to fully mix the materials, performing hydrothermal reaction on the solution at 160-180 ℃ for 12-24 hours to obtain a polypyrrole/graphene composite material solution, performing centrifugal separation on the composite material solution, washing with water, and drying to obtain the polypyrrole/graphene composite material, wherein the mass ratio of graphene to polypyrrole is 1:3 to 80.8;
(6) dispersing the polypyrrole/graphene composite material prepared in the step (5) into water, wherein the concentration of a composite material water solution is 1-10 mg/mL; and (3) the solution is coated on the surface of the ceramic wafer substrate with the carbon interdigital electrode obtained in the step (2) in a suspension manner, and then heat treatment is carried out for 1-4 hours at the temperature of 80-130 ℃, so that the thickness of the obtained sensitive film is 10-30 mu m, and the polypyrrole/graphene composite material-based resistance type gas sensor is prepared.
2. Polypyrrole/graphene composite material-based resistance type NH3A sensor, characterized by: is prepared by the method of claim 1.
3. The polypyrrole/graphene composite material-based resistive NH according to claim 23Sensor at NH3Application in detection.
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