CN105891271B - It is a kind of based on graphene/resistor-type gas sensor of stannic oxide/zinc oxide composite, preparation method and applications - Google Patents
It is a kind of based on graphene/resistor-type gas sensor of stannic oxide/zinc oxide composite, preparation method and applications Download PDFInfo
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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
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- 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
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- 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
Abstract
It is a kind of based on graphene/resistor-type gas sensor of stannic oxide/zinc oxide composite, preparation method and applications, belong to gas sensor technical field.It is made of successively monocrystalline substrate, silicon dioxide layer, titanium adhesion layer, interdigital platinum electrode, the gas-sensitive film that is coated in silicon dioxide layer and interdigital platinum electrode surface；Titanium adhesion layer is identical as the structure of interdigital platinum electrode, and gas-sensitive film is graphene/stannic oxide/zinc oxide trielement composite material；The trielement composite material is mixed by graphene, stannic oxide and zinc oxide, is three-dimensional porous structure.Before and after gas-sensitive film contact measured gas, resistance can change, and by the variation of resistance between the interdigital platinum electrode of measurement, can obtain the sensitivity of sensor.The sensor has very high response sensitivity, quickly response regeneration rate and good response invertibity at room temperature, solves the problems, such as that stannic oxide and zinc oxide gas sensor needs could work at high temperature.
Description
Technical field
The invention belongs to gas sensor technical fields, and in particular to a kind of graphene with room temperature air-sensitive response characteristic
Based resistance type gas sensor and preparation method thereof, it is compound based on graphene/stannic oxide/zinc oxide more particularly to one kind
The resistor-type gas sensor of material, preparation method and applications.
Background technology
With the fast development of industrial or agricultural and transportation, problem of environmental pollution is more and more prominent.Especially in recent years
Toxic and harmful gas, flammable explosive gas discharge capacity increasingly increase, to the gas in environment carry out accurate, continuous detection at
For urgent problem to be solved, this just provides wide space for the application of gas sensor.Gas sensor is a kind of important
Chemical sensor, have a wide range of applications in the fields such as industrial and agricultural production, process control, environmental monitoring and protection and anti-terrorism.
Developing has many advantages, such as high sensitivity, low cost, low-power consumption, the high performance gas sensor that minimizes as scientific research field and production
The research hotspot of industry.Wherein, sensitive material is the core of gas sensor, and the key for improving gas sensor performance is exploitation
Gas sensitive with excellent response characteristic.
Currently, becoming the most widely used a kind of sensitive as the conductor oxidate of representative using stannic oxide, zinc oxide
Material has many advantages, such as that preparation is convenient, of low cost, derives from a wealth of sources, but there is also some shortcomings simultaneously, for example, stability
It is poor, it is affected by humidity, selectivity is not ideal enough etc..The gas sensor for being based particularly on metal oxide is required for
It works at higher temperature, this makes the power consumption of element larger, it is difficult to prepare portable instrument.Operating temperature high simultaneously is direct
The stability of sensor is influenced, nor can be used in the environment there are flammable explosive gas, makes its application by certain
Limitation.
In order to solve this problem, the operating temperature for reducing sensor, the gas sensitive for developing working and room temperature are studied
The extensive concern of person.Researchers' trial prepares the composite material of metal oxide and conducting polymer, and development can working and room temperature
Gas sensor.Although realizing room temperature detection gas, metal oxide is shown with conducting polymer composite material
Sensitivity is low, response restores the problems such as slow, seriously it is hindered further to apply.In recent years, using graphene as the Two-dimensional Carbon of representative
Based nano-material is quickly grown, and becomes the hot spot of material circle research.The conductivity at room temperature and fast carrier that graphene has move
Shifting rate provides new thinking to develop the gas sensitive of working and room temperature.Research finds that room temperature may be implemented in grapheme material really
Detection gas.In addition, graphene and the compound spirit that graphene-based gas sensor can be further improved of conductor oxidate
Sensitivity improves response regeneration rate, or even is expected to realize highly sensitive gas detection at room temperature.Develop graphene-based room temperature air
Sensor becomes one of the important directions of sensor field research, and development is very fast.
Invention content
The object of the present invention is to provide a kind of graphene/titanium dioxides at room temperature with highly sensitive gas response characteristic
The resistor-type gas sensor of tin/zinc oxide composite, preparation method and applications.
A kind of resistor-type gas sensor based on graphene/stannic oxide/zinc oxide composite of the present invention,
It is characterized in that：Successively by monocrystalline substrate, silicon dioxide layer, titanium adhesion layer, interdigital platinum electrode, in silicon dioxide layer and interdigital
The gas-sensitive film composition of platinum electrode surface coating；Titanium adhesion layer is identical as the structure of interdigital platinum electrode, gas-sensitive film
For graphene/stannic oxide/zinc oxide trielement composite material；Its resistance can occur before and after gas-sensitive film contact measured gas
Variation can obtain the sensitivity of sensor by the variation of resistance between the interdigital platinum electrode of measurement.
Graphene/stannic oxide/zinc oxide the trielement composite material, is mixed by graphene, stannic oxide and zinc oxide
It closes, mass ratio 1：5~100：1~50, trielement composite material is three-dimensional porous structure, and pore size is 3~10nm,
BET specific surface area is 100~230m2/g。
Further, the thickness of silicon dioxide layer is 150~300nm, and the thickness of titanium adhesion layer is 40~90 nm, platinum
The thickness for belonging to layer, that is, interdigital platinum electrode is 50~200nm, and the logarithm of electrode is 4~6 pairs, and the width of electrode is 50~100 μm, electricity
Spacing between pole refers to is 50~100 μm, is connected on interdigital platinum electrode leaded；The thickness of gas-sensitive film is 10~50 μ
m。
The preparation of graphene/stannic oxide of the present invention/zinc oxide trielement composite material resistor-type gas sensor
Method, its step are as follows：
(1) using monocrystalline silicon as substrate, using thermal oxidation method monocrystalline silicon surface prepare silicon dioxide layer, thickness be 150~
300nm；Using magnetron sputtering method in the surface titanium deposition adhesion layer of silica, thickness is 40~90nm；Utilize magnetron sputtering
Method sticks layer surface in titanium and deposits platinum metal layer, and thickness is 50~200nm；In platinum metal surface spin coating photoresist, thickness 1
~2 μm；Photolithography plate identical with interdigital platinum electrode figure is placed on photoresist surface, is divided in the exposed under UV light 15 of 350W
Then clock is developed with sodium hydroxide solution, the photoresist exposed after development is removed；Recycle argon ion bombardment platinum
Layer and titanium stick layer surface, and the platinum metal layer and titanium adhesion layer for not being photo-etched glue cover are removed, then clear with ethanol solution
Unexposed photoresist is washed off, to the titanium adhesion layer for obtaining interdigitated electrode structure and interdigital platinum electrode, the logarithm of electrode is 4~
6 pairs, the width of electrode is 50~100 μm, and the spacing between electrode finger is 50~100 μm.
(2) it is cleaned by ultrasonic surface successively with ethyl alcohol, water and prepares the monocrystalline substrate for having interdigital platinum electrode, drying；
(3) preparation graphene oxide water solution, the mg/mL of a concentration of 0.1mg/mL~5 of graphene oxide water solution, so
After be added butter of tin, ultrasonic disperse keeps its mixing abundant, and the quality amount ratio of graphene oxide, butter of tin and water is 1：10
~200：5000~100000；By above-mentioned solution under the conditions of 160~180 DEG C hydro-thermal reaction 12~24 hours, be made graphite
Composite material solution is centrifuged, washed and dried, obtains graphene/stannic oxide by alkene/tin dioxide composite material solution
Composite material；Graphene/tin dioxide composite material is added in methanol, the quality amount ratio of graphene and methanol is 1：
4000~200000；Then be added zinc nitrate and potassium hydroxide, graphene, stannic oxide, zinc nitrate and potassium hydroxide weight
Than being 1：5~100：2~150：4~300, stirring and ultrasound make it be uniformly dispersed；Above-mentioned solution is put into oil bath 60~
It is reacted 1~12 hour at 80 DEG C, graphene/stannic oxide/zinc oxide trielement composite material solution is made；By above-mentioned solution into
Row is centrifuged, washes and is dried, and obtains graphene/stannic oxide/zinc oxide trielement composite material.
(4) graphene/stannic oxide/zinc oxide trielement composite material prepared by step (3) is distributed in water, composite wood
Expect a concentration of 1~10mg/mL of aqueous solution；The solution is coated with the monocrystalline silicon with interdigital platinum electrode that step (2) obtains
Then substrate surface is heat-treated 1~4 hour at 80~130 DEG C, the thickness of obtained sensitive thin film is 10~50 μm, to
The resistor-type gas sensor based on graphene/stannic oxide/zinc oxide composite is made.
Gas sensor prepared by the present invention is used for NO2Room temperature response, a concentration of 1~100 ppm of nitrogen dioxide,
It is preferably 1~5ppm.
It is an advantage of the invention that：
1) titanium adhesion layer is added between silica and interdigital platinum electrode, improves interdigital platinum electrode and silicon dioxide substrates
Adhesive force improves the stability of device.
2) in composite material stannic oxide and zinc oxide introducing, can further prevent the reunion of graphene sheet layer,
Effectively improve the specific surface area of composite material.Prepared graphene/stannic oxide/zinc oxide composite has three-dimensional more
Pore structure, big specific surface area so that sensor has very high response sensitivity, quickly responds regeneration rate at room temperature
With good response invertibity, solve stannic oxide and zinc oxide gas sensor usually require it is just workable at high temperature
Problem.
3) graphene/stannic oxide/zinc oxide composite being prepared using wet chemistry method, method is simple, easily operated, at
This is cheap.And it can realize stone by experiment parameters such as the ratios of controlling reaction temperature, reaction time and pre-reaction material
The regulation and control of the performances such as composition, the structure of mertenyl composite material.
4) in composite material graphene introducing, the electric conductivity of sensitive material can be significantly increased, avoid usual dioxy
Change tin and zinc oxide because room temperature resistance is excessively high, response sensitivity is extremely low and cannot achieve room temperature detection gas.
5) stannic oxide and two kinds of Nanoparticle Modifieds of zinc oxide are on the surface of graphene in composite material, by titanium dioxide
The tin surface-active site different with zinc oxide realizes that the regulation and control of surface double activated site promote the sensitive property of sensor.
6) in composite material stannic oxide and zinc oxide introducing, it includes stone that can form a variety of heterojunction structures in the material
Heterojunction structure between black alkene and stannic oxide and zinc oxide semi-conductor, the heterojunction structure between stannic oxide and zinc oxide, regulation and control
The semiconducting behavior and structure feature of graphene, realize the promotion of sensor performance.
7) wet chemistry method in-situ preparation stannic oxide and zinc oxide nano-particle on the surface of graphene are used, it can be significantly
The combination for improving stannic oxide and zinc oxide and carbon-based material, improves the conductivity at room temperature of material, is advantageously implemented room temperature detection
Gas.The composite material solution of preparation may be used the methods of spin coating and form a film in interdigital electrode, easy to process, can be easily
Gas sensor is prepared, traditional metal-oxide gas transducer is solved and needs high temperature sintering, processes complicated problem.
Description of the drawings
Fig. 1 is the structural schematic diagram of the gas sensor of the present invention.
Wherein：Monocrystalline silicon 1, silicon dioxide layer 2, titanium adhesion layer 3, interdigital platinum electrode 4, gas-sensitive film 5, lead 6,
7。
Fig. 2 is the X-ray diffraction spectrogram of graphene/stannic oxide/zinc oxide composite.
Fig. 3 is graphene/stannic oxide/zinc oxide composite gas sensor to 5ppm NO2Room temperature dynamic response
Recovery curve.
Fig. 4 is graphene/stannic oxide/zinc oxide composite gas sensor to 5ppm NO2Room temperature response it is sensitive
(sensitivity definition is sensor in air and in NO to degree2In gas, the ratio of resistance between interdigital platinum electrode) with gas concentration
Change curve.
Fig. 5 is graphene/stannic oxide/zinc oxide composite gas sensor to 5ppm NO2Room temperature response weight
Renaturation curve.
Specific implementation mode
It is further illustrated the present invention below in conjunction with drawings and examples.
Embodiment 1
(1) using monocrystalline silicon as substrate, silicon dioxide layer is generated in monocrystalline silicon surface using thermal oxidation method, thickness is
150nm, using magnetron sputtering method in the surface titanium deposition adhesion layer of silica, thickness is 40 nm；Existed using magnetron sputtering method
Titanium sticks layer surface deposition platinum metal layer, thickness 50nm；In platinum metal surface spin coating BP212 (Kempur
Microelectronic INC) positive photoresist, thickness is 1 μm；Photolithography plate identical with interdigital platinum electrode figure is placed on light
Then use the sodium hydroxide solution that mass fraction is 5/1000ths aobvious in the exposed under UV light 15 minutes of 350W in photoresist surface
Shadow, the photoresist exposed after development are removed；Argon ion bombardment platinum metal layer and titanium is recycled to stick layer surface, not by light
The platinum metal layer and titanium adhesion layer that photoresist is covered are removed；Then unexposed photoresist is washed with ethanol solution, to
The titanium adhesion layer of interdigital platinum electrode and interdigitated electrode structure is obtained, the logarithm of interdigital platinum electrode is 4 pairs, and the width of electrode is 50 μ
M, the spacing between electrode finger are 50 μm.
(2) it is substrate to be cleaned by ultrasonic surface successively to be printed on the monocrystalline silicon of interdigital platinum electrode with ethyl alcohol, water, and drying is for use；
(3) graphene oxide water solution for preparing a concentration of 0.1mg/mL of 1mL, adds graphene oxide into aqueous solution
In, butter of tin is then added, ultrasonic disperse keeps its mixing abundant, and the weight ratio of graphene oxide, butter of tin and water is 1：
10：5000；By above-mentioned solution, hydro-thermal reaction 24 hours, obtained graphene/tin dioxide composite material solution are incited somebody to action at 180 DEG C
Above-mentioned solution is centrifuged, washes and dries, and obtains graphene/tin dioxide composite material；By graphene/stannic oxide
Into methanol solution, the weight ratio of graphene and methanol is 1：4000；Then zinc nitrate and potassium hydroxide, graphene, two are added
The weight ratio of tin oxide, zinc nitrate and potassium hydroxide is 1：5：2：4, stirring and ultrasound make it be uniformly dispersed；Above-mentioned solution is put
To being reacted 12 hours at 60 DEG C in oil bath, graphene/stannic oxide/zinc oxide trielement composite material solution is made；It will be above-mentioned
Solution is centrifuged, washes, dries, and obtains graphene/stannic oxide/zinc oxide trielement composite material, and product quality is
240mg。
Graphene in obtained trielement composite material：Stannic oxide：The weight ratio of zinc oxide is 1： 5：1, ternary is multiple
Condensation material is three-dimensional porous structure, pore size 3nm, BET specific surface area 100m2/g。
(4) graphene/stannic oxide/zinc oxide trielement composite material prepared by step (3) is distributed in water, prepares stone
The aqueous solution of black alkene/stannic oxide/zinc oxide trielement composite material, a concentration of 1mg/mL of composite material；Above-mentioned solution is hanged
It is coated onto the surface of silicon with interdigital platinum electrode of step (2), is heat-treated at 80 DEG C 4 hours and obtains sensitive material film,
The thickness of film is 10 μm, and the resistor-type gas sensor based on graphene/stannic oxide/zinc oxide composite is made.
Embodiment 2
(1) using monocrystalline silicon as substrate, silicon dioxide layer is generated in monocrystalline silicon surface using thermal oxidation method, thickness is
180nm, using magnetron sputtering method in the surface titanium deposition adhesion layer of silica, thickness is 60 nm；Existed using magnetron sputtering method
Titanium sticks layer surface deposition platinum metal layer, thickness 100nm；In platinum metal surface spin coating BP212 (Kempur
Microelectronic INC) positive photoresist, thickness is 1 μm；Photolithography plate identical with interdigital platinum electrode figure is placed on light
Then use the sodium hydroxide solution that mass fraction is 5/1000ths aobvious in the exposed under UV light 15 minutes of 350W in photoresist surface
Shadow, the photoresist exposed after development are removed；Then argon ion bombardment platinum metal layer and titanium is recycled to stick layer surface, not
The platinum metal layer and titanium adhesion layer for being photo-etched glue cover are removed；Then unexposed photoresist is washed with ethanol solution,
To obtain the titanium adhesion layer of interdigital platinum electrode and interdigitated electrode structure, interdigital platinum electrode is obtained, the logarithm of electrode is 4 pairs, electricity
The width of pole is 70 μm, and the spacing between electrode finger is 50 μm.
(2) it is substrate to be cleaned by ultrasonic surface successively to be printed on the monocrystalline silicon of interdigital platinum electrode with ethyl alcohol, water, and drying is for use；
(3) graphene oxide water solution for preparing a concentration of 0.5mg/mL of 1mL, adds graphene oxide into aqueous solution
In, butter of tin is then added, ultrasonic disperse keeps its mixing abundant, and the weight ratio of graphene oxide, butter of tin and water is 1：
50：1000；By above-mentioned solution, hydro-thermal reaction 18 hours, obtained graphene/tin dioxide composite material solution are incited somebody to action at 160 DEG C
Above-mentioned solution is centrifuged, washes and dries, and obtains graphene/tin dioxide composite material；By graphene/stannic oxide
Into methanol solution, the weight ratio of graphene and methanol is 1：5000；Then zinc nitrate and potassium hydroxide, graphene, two are added
The weight ratio of tin oxide, zinc nitrate and potassium hydroxide is 1：10：25：50, stirring and ultrasound make it be uniformly dispersed；By above-mentioned solution
It is put into oil bath and is reacted 8 hours at 60 DEG C, graphene/stannic oxide/zinc oxide trielement composite material solution is made；It will be above-mentioned
Solution is centrifuged, washes, dries, and obtains graphene/stannic oxide/zinc oxide trielement composite material, and product quality is
280mg。
Graphene in obtained trielement composite material：Stannic oxide：The weight ratio of zinc oxide is 1： 10：5, ternary
Composite material is three-dimensional porous structure, pore size 5nm, BET specific surface area 150m2/g。
(4) graphene/stannic oxide/zinc oxide trielement composite material prepared by step (3) is distributed in water, prepares stone
The aqueous solution of black alkene/stannic oxide/zinc oxide trielement composite material, a concentration of 2mg/mL of composite material；Above-mentioned solution is hanged
It is coated onto the surface of silicon with interdigital platinum electrode of step (2), is heat-treated at 80 DEG C 2 hours and obtains sensitive material film,
The thickness of film is 20 μm, and the resistor-type gas sensor based on graphene/stannic oxide/zinc oxide composite is made.
Embodiment 3
(1) using monocrystalline silicon as substrate, silicon dioxide layer is generated in monocrystalline silicon surface using thermal oxidation method, thickness is
210nm, using magnetron sputtering method in the surface titanium deposition adhesion layer of silica, thickness is 60 nm；Existed using magnetron sputtering method
Titanium sticks layer surface deposition platinum metal layer, thickness 100nm；In platinum metal surface spin coating BP212 (Kempur
Microelectronic INC) positive photoresist, thickness is 1 μm；Photolithography plate identical with interdigital platinum electrode figure is placed on light
Then use the sodium hydroxide solution that mass fraction is 5/1000ths aobvious in the exposed under UV light 15 minutes of 350W in photoresist surface
Shadow, the photoresist exposed after development are removed；Then argon ion bombardment platinum metal layer and titanium is recycled to stick layer surface, not
The platinum metal layer and titanium adhesion layer for being photo-etched glue cover are removed；Then unexposed photoresist is washed with ethanol solution,
To obtain the titanium adhesion layer of interdigital platinum electrode and interdigitated electrode structure, interdigital platinum electrode is obtained, the logarithm of electrode is 5 pairs, electricity
The width of pole is 70 μm, and the spacing between electrode finger is 80 μm.
(2) it is substrate to be cleaned by ultrasonic surface successively to be printed on the monocrystalline silicon of interdigital platinum electrode with ethyl alcohol, water, and drying is for use；
(3) graphene oxide water solution for preparing a concentration of 1mg/mL of 1mL, adds graphene oxide into aqueous solution,
Then butter of tin is added, ultrasonic disperse keeps its mixing abundant, and the weight ratio of graphene oxide, butter of tin and water is 1：50：
10000；By at 170 DEG C hydro-thermal reaction 18 hours, be made graphene/tin dioxide composite material solution, by above-mentioned solution
It is centrifuged, washes and dries, obtain graphene/tin dioxide composite material；Graphene/stannic oxide is molten to methanol
In liquid, the weight ratio of graphene and methanol is 1：10000；Then be added zinc nitrate and potassium hydroxide, graphene, stannic oxide,
The weight ratio of zinc nitrate and potassium hydroxide is 1：25：50：100, stirring and ultrasound make it be uniformly dispersed；Above-mentioned solution is put into oil
It is reacted 12 hours at 70 DEG C in bath, graphene/stannic oxide/zinc oxide trielement composite material solution is made；By above-mentioned solution
It is centrifuged, washes, dries, obtain graphene/stannic oxide/zinc oxide trielement composite material, product quality is
300mg。
Graphene in obtained trielement composite material：Stannic oxide：The weight ratio of zinc oxide is 1：25：10, ternary
Composite material is three-dimensional porous structure, pore size 7nm, BET specific surface area 180m2/g。
(4) graphene/stannic oxide/zinc oxide trielement composite material prepared by step (3) is distributed in water, prepares stone
The aqueous solution of black alkene/stannic oxide/zinc oxide trielement composite material, a concentration of 4mg/mL of composite material；Above-mentioned solution is hanged
It is coated onto the surface of silicon with interdigital platinum electrode of step (2), is heat-treated at 90 DEG C 4 hours and obtains sensitive material film,
The thickness of film is 30 μm, and the resistor-type gas sensor based on graphene/stannic oxide/zinc oxide composite is made.
Embodiment 4
(1) using monocrystalline silicon as substrate, silicon dioxide layer is generated in monocrystalline silicon surface using thermal oxidation method, thickness is
240nm, using magnetron sputtering method in the surface titanium deposition adhesion layer of silica, thickness is 80 nm；Existed using magnetron sputtering method
Titanium sticks layer surface deposition platinum metal layer, thickness 150nm；In platinum metal surface spin coating BP212 (Kempur
Microelectronic INC) positive photoresist, thickness is 2 μm；Photolithography plate identical with interdigital platinum electrode figure is placed on light
Then use the sodium hydroxide solution that mass fraction is 5/1000ths aobvious in the exposed under UV light 15 minutes of 350W in photoresist surface
Shadow, the photoresist exposed after development are removed；Then argon ion bombardment platinum metal layer and titanium is recycled to stick layer surface, not
The platinum metal layer and titanium adhesion layer for being photo-etched glue cover are removed；Then unexposed photoresist is washed with ethanol solution,
To obtain the titanium adhesion layer of interdigital platinum electrode and interdigitated electrode structure, interdigital platinum electrode is obtained, the logarithm of electrode is 5 pairs, electricity
The width of pole is 80 μm, and the spacing between electrode finger is 80 μm.
(2) it is substrate to be cleaned by ultrasonic surface successively to be printed on the monocrystalline silicon of interdigital platinum electrode with ethyl alcohol, water, and drying is for use；
(3) graphene oxide water solution for preparing a concentration of 1.5mg/mL of 1mL, adds graphene oxide into aqueous solution
In, butter of tin is then added, ultrasonic disperse keeps its mixing abundant, and the weight ratio of graphene oxide, butter of tin and water is 1：
100：50000；By above-mentioned solution at 170 DEG C hydro-thermal reaction 16 hours, be made graphene/tin dioxide composite material solution,
Above-mentioned solution is centrifuged, washed and dried, graphene/tin dioxide composite material is obtained；By graphene/titanium dioxide
In tin to methanol solution, the weight ratio of graphene and methanol is 1：50000；Then addition zinc nitrate and potassium hydroxide, graphene,
The weight ratio of stannic oxide, zinc nitrate and potassium hydroxide is 1：50：75：150, stirring and ultrasound make it be uniformly dispersed；It will be above-mentioned
Solution is put into oil bath to react 8 hours at 70 DEG C, and graphene/stannic oxide/zinc oxide trielement composite material solution is made；
Above-mentioned solution is centrifuged, wash, is dried, graphene/stannic oxide/zinc oxide trielement composite material, product are obtained
Quality is 320mg.
Graphene in obtained trielement composite material：Stannic oxide：The weight ratio of zinc oxide is 1： 50：15, ternary
Composite material is three-dimensional porous structure, pore size 8nm, BET specific surface area 200m2/g。
(4) graphene/stannic oxide/zinc oxide trielement composite material prepared by step (3) is distributed in water, prepares stone
The aqueous solution of black alkene/stannic oxide/zinc oxide trielement composite material, a concentration of 6mg/mL of composite material；Above-mentioned solution is hanged
It is coated onto the surface of silicon with interdigital platinum electrode of step (2), is heat-treated at 100 DEG C 3 hours and obtains sensitive material film,
The thickness of film is 30 μm, and the resistor-type gas sensor based on graphene/stannic oxide/zinc oxide composite is made.
Embodiment 5
(1) using monocrystalline silicon as substrate, silicon dioxide layer is generated in monocrystalline silicon surface using thermal oxidation method, thickness is
270nm, using magnetron sputtering method in the surface titanium deposition adhesion layer of silica, thickness is 80 nm；Existed using magnetron sputtering method
Titanium sticks layer surface deposition platinum metal layer, thickness 150nm；In platinum metal surface spin coating BP212 (Kempur
Microelectronic INC) positive photoresist, thickness is 2 μm；Photolithography plate identical with interdigital platinum electrode figure is placed on light
Then use the sodium hydroxide solution that mass fraction is 5/1000ths aobvious in the exposed under UV light 15 minutes of 350W in photoresist surface
Shadow, the photoresist exposed after development are removed；Then argon ion bombardment platinum metal layer and titanium is recycled to stick layer surface, not
The platinum metal layer and titanium adhesion layer for being photo-etched glue cover are removed；Then unexposed photoresist is washed with ethanol solution,
To obtain the titanium adhesion layer of interdigital platinum electrode and interdigitated electrode structure, interdigital platinum electrode is obtained, the logarithm of electrode is 5 pairs, electricity
The width of pole is 90 μm, and the spacing between electrode finger is 100 μm.
(2) it is substrate to be cleaned by ultrasonic surface successively to be printed on the monocrystalline silicon of interdigital platinum electrode with ethyl alcohol, water, and drying is for use；
(3) graphene oxide water solution for preparing a concentration of 3mg/mL of 1mL, adds graphene oxide into aqueous solution,
Then butter of tin is added, ultrasonic disperse keeps its mixing abundant, and the weight ratio of graphene oxide, butter of tin and water is 1：100：
50000；By above-mentioned solution at 180 DEG C hydro-thermal reaction 16 hours, be made graphene/tin dioxide composite material solution, will be upper
It states solution to be centrifuged, wash and dry, obtains graphene/tin dioxide composite material；Graphene/stannic oxide is arrived
In methanol solution, the weight ratio of graphene and methanol is 1：100000；Then zinc nitrate and potassium hydroxide, graphene, two are added
The weight ratio of tin oxide, zinc nitrate and potassium hydroxide is 1：75：100：200, stirring and ultrasound make it be uniformly dispersed；It will be above-mentioned
Solution is put into oil bath to react 8 hours at 80 DEG C, and graphene/stannic oxide/zinc oxide trielement composite material solution is made；
Above-mentioned solution is centrifuged, wash, is dried, graphene/stannic oxide/zinc oxide trielement composite material, product are obtained
Quality is 340mg.
Graphene in obtained trielement composite material：Stannic oxide：The weight ratio of zinc oxide is 1： 75：25, ternary
Composite material is three-dimensional porous structure, pore size 10nm, BET specific surface area 210m2/g。
(4) graphene/stannic oxide/zinc oxide trielement composite material prepared by step (3) is distributed in water, prepares stone
The aqueous solution of black alkene/stannic oxide/zinc oxide trielement composite material, a concentration of 8mg/mL of composite material；Above-mentioned solution is hanged
It is coated onto the surface of silicon with interdigital platinum electrode of step (2), is heat-treated at 110 DEG C 2 hours and obtains sensitive material film,
The thickness of film is 40 μm, and the resistor-type gas sensor based on graphene/stannic oxide/zinc oxide composite is made.
Embodiment 6
(1) using monocrystalline silicon as substrate, silicon dioxide layer is generated in monocrystalline silicon surface using thermal oxidation method, thickness is
300nm, using magnetron sputtering method in the surface titanium deposition adhesion layer of silica, thickness is 90 nm；Existed using magnetron sputtering method
Titanium sticks layer surface deposition platinum metal layer, thickness 200nm；In platinum metal surface spin coating BP212 (Kempur
Microelectronic INC) positive photoresist, thickness is 2 μm；Photolithography plate identical with interdigital platinum electrode figure is placed on light
Then use the sodium hydroxide solution that mass fraction is 5/1000ths aobvious in the exposed under UV light 15 minutes of 350W in photoresist surface
Shadow, the photoresist exposed after development are removed；Then argon ion bombardment platinum metal layer and titanium is recycled to stick layer surface, not
The platinum metal layer and titanium adhesion layer for being photo-etched glue cover are removed；Then unexposed photoresist is washed with ethanol solution,
To obtain the titanium adhesion layer of interdigital platinum electrode and interdigitated electrode structure, interdigital platinum electrode is obtained, the logarithm of electrode is 6 pairs, electricity
The width of pole is 90 μm, and the spacing between electrode finger is 100 μm.
(2) it is substrate to be cleaned by ultrasonic surface successively to be printed on the monocrystalline silicon of interdigital platinum electrode with ethyl alcohol, water, and drying is for use；
(3) graphene oxide water solution for preparing a concentration of 5mg/mL of 1mL, adds graphene oxide into aqueous solution,
Then butter of tin is added, ultrasonic disperse keeps its mixing abundant, and the weight ratio of graphene oxide, butter of tin and water is 1：200：
100000；By above-mentioned solution at 180 DEG C hydro-thermal reaction 12 hours, be made graphene/tin dioxide composite material solution, will be upper
It states solution to be centrifuged, wash and dry, obtains graphene/tin dioxide composite material；Graphene/stannic oxide is arrived
In methanol solution, the weight ratio of graphene and methanol is 1：200000；Then zinc nitrate and potassium hydroxide, graphene, two are added
The weight ratio of tin oxide, zinc nitrate and potassium hydroxide is 1：100： 150：300, stirring and ultrasound make it be uniformly dispersed；It will be above-mentioned
Solution is put into oil bath to react 1 hour at 80 DEG C, and graphene/stannic oxide/zinc oxide trielement composite material solution is made；It will
Above-mentioned solution is centrifuged, washes, dries, and obtains graphene/stannic oxide/zinc oxide trielement composite material, product matter
Amount is 360mg.
Graphene in obtained trielement composite material：Stannic oxide：The weight ratio of zinc oxide is 1： 100：50, three
First composite material is three-dimensional porous structure, pore size 10nm, BET specific surface area 230m2/g。
(4) graphene/stannic oxide/zinc oxide trielement composite material prepared by step (3) is distributed in water, prepares stone
The aqueous solution of black alkene/stannic oxide/zinc oxide trielement composite material, a concentration of 10mg/mL of composite material；By above-mentioned solution
It is coated with the surface of silicon with interdigital platinum electrode of step (2), it is thin that 1 hour acquisition sensitive material is heat-treated at 130 DEG C
The thickness of film, film is 50 μm, and the resistor-type gas sensor based on graphene/stannic oxide/zinc oxide composite is made.
Graphene/stannic oxide/zinc oxide trielement composite material X-ray diffraction spectrogram such as Fig. 2 institutes prepared by embodiment 1
Show, as seen from Figure 2, composite material has the diffraction maximum for typically belonging to stannic oxide and zinc oxide, illustrates composite wood
Material is containing by two kinds of metal oxides of stannic oxide and oxidisability.
Gas sensor based on graphene/stannic oxide/zinc oxide trielement composite material prepared by embodiment 1 is in room temperature
Under Fig. 3 is shown in the response recovery curve of various concentration nitrogen dioxide.As can be seen that the graphene-based gas sensor prepared is not to
With concentration nitrogen dioxide have response very high, quickly, the response time be less than 1 minute, and sensor have well may be used
Inverse property.
Gas sensor based on graphene/stannic oxide/zinc oxide trielement composite material prepared by embodiment 1 is to difference
The response sensitivity curve of concentration nitrogen dioxide is shown in Fig. 4.As can be seen that sensor at room temperature has the nitrogen dioxide of low concentration
There is higher sensitivity, 1.5 are reached for 1ppm nitrogen dioxide.
Gas sensor based on graphene/stannic oxide/zinc oxide trielement composite material prepared by embodiment 1 is in room temperature
Under linearity curve repeated to the response of 5ppm nitrogen dioxide see Fig. 5.As can be seen that it is multiple to pass through nitrogen dioxide-air at room temperature
Loop test, response curve is almost unchanged, shows that the sensor has good response repeatability.
Claims (6)
1. a kind of resistor-type gas sensor based on graphene/stannic oxide/zinc oxide composite, is served as a contrast by monocrystalline silicon successively
Bottom, silicon dioxide layer, titanium adhesion layer, interdigital electrode, the gas-sensitive film coated in silicon dioxide layer and interdigital electrode surface
Composition, titanium adhesion layer are identical as the structure of interdigital electrode；It is characterized in that：Interdigital electrode is platinum electrode, and gas-sensitive film is
Graphene/stannic oxide/zinc oxide trielement composite material；The trielement composite material is mixed by graphene, stannic oxide and zinc oxide
It closes, mass ratio 1：5~100：1~50, trielement composite material is three-dimensional porous structure, and pore size is 3~10nm,
BET specific surface area is 100~230m2/g。
2. a kind of resistor-type gas sensing based on graphene/stannic oxide/zinc oxide composite as described in claim 1
Device, it is characterised in that：The thickness of silicon dioxide layer is 150~300nm, and the thickness of titanium adhesion layer is 40~90nm, platinum metal layer
The thickness of i.e. interdigital platinum electrode is 50~200nm, and the logarithm of electrode is 4~6 pairs, and the width of electrode is 50~100 μm, electrode finger
Between spacing be 50~100 μm, the thickness of gas-sensitive film is 10~50 μm.
3. a kind of resistor-type gas sensor based on graphene/stannic oxide/zinc oxide composite described in claim 1
Preparation method, its step are as follows：
(1) using monocrystalline silicon as substrate, silicon dioxide layer is prepared in monocrystalline silicon surface using thermal oxidation method；Existed using magnetron sputtering method
The surface titanium deposition adhesion layer of silica；Stick layer surface in titanium using magnetron sputtering method and deposits platinum metal layer；In platinum
Surface spin coating photoresist, thickness are 1~2 μm；Photolithography plate identical with interdigital platinum electrode figure is placed on photoresist surface, it is ultraviolet
It exposes under light, is then developed with sodium hydroxide solution, the photoresist exposed after development is removed；Recycle argon ion bombardment
Platinum metal layer and titanium stick layer surface, and the platinum metal layer and titanium adhesion layer for not being photo-etched glue cover are removed, and then use ethyl alcohol
Solution washes unexposed photoresist, to the titanium adhesion layer for obtaining interdigitated electrode structure and interdigital platinum electrode；
(2) it is cleaned by ultrasonic surface successively with ethyl alcohol, water and prepares the monocrystalline substrate for having interdigital platinum electrode, drying；
(3) graphene oxide water solution is prepared, then a concentration of 0.1mg/mL~5mg/mL of graphene oxide water solution is added
Butter of tin, ultrasonic disperse keep its mixing abundant, and the quality amount ratio of graphene oxide, butter of tin and water is 1：10~200：
5000~100000；By above-mentioned solution under the conditions of 160~180 DEG C hydro-thermal reaction 12~24 hours, be made graphene/titanium dioxide
Composite material solution is centrifuged, washed and dried, obtains graphene/tin dioxide composite material by tin composite material solution；
Graphene/tin dioxide composite material is added in methanol, the quality amount ratio of graphene and methanol is 1：4000~
200000；Then be added zinc nitrate and potassium hydroxide, graphene, stannic oxide, zinc nitrate and potassium hydroxide weight ratio be 1：5
~100：2~150：4~300, stirring and ultrasound make it be uniformly dispersed；Above-mentioned solution is put into oil bath at 60~80 DEG C instead
It answers 1~12 hour, graphene/stannic oxide/zinc oxide trielement composite material solution is made；Above-mentioned solution is subjected to centrifugation point
From, washing and drying, obtain graphene/stannic oxide/zinc oxide trielement composite material；
(4) graphene/stannic oxide/zinc oxide trielement composite material prepared by step (3) is distributed in water, composite material water
A concentration of 1~10mg/mL of solution；The solution is coated with the monocrystalline substrate with interdigital platinum electrode that step (2) obtains
Then surface is heat-treated 1~4 hour at 80~130 DEG C, graphene/stannic oxide/zinc oxide composite wood is based on to be made
The resistor-type gas sensor of material.
4. a kind of resistor-type gas based on graphene/stannic oxide/zinc oxide composite as claimed in claim 1 or 2 passes
Sensor is in detection NO2In application.
5. a kind of resistor-type gas sensing based on graphene/stannic oxide/zinc oxide composite as claimed in claim 4
Device is in detection NO2In application, it is characterised in that：NO2A concentration of 1~100ppm.
6. a kind of resistor-type gas sensing based on graphene/stannic oxide/zinc oxide composite as claimed in claim 5
Device is in detection NO2In application, it is characterised in that：NO2A concentration of 1~5ppm.
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