CN105891271A - Resistance-type gas sensor based on graphene, stannic oxide and zinc oxide composite, preparation method and application thereof - Google Patents
Resistance-type gas sensor based on graphene, stannic oxide and zinc oxide composite, preparation method and application thereof Download PDFInfo
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- CN105891271A CN105891271A CN201610195240.0A CN201610195240A CN105891271A CN 105891271 A CN105891271 A CN 105891271A CN 201610195240 A CN201610195240 A CN 201610195240A CN 105891271 A CN105891271 A CN 105891271A
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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
The invention relates to a resistance-type gas sensor based on a graphene, stannic oxide and zinc oxide composite, a preparation method and application thereof, and belongs to the technical field of gas sensors. The gas sensor is composed of a monocrystalline silicon substrate, a silicon dioxide layer, a titanium adhesion layer, interdigital platinum electrodes and a gas sensitive film covering the silicon dioxide layer and the surfaces of the interdigital platinum electrodes in sequence; the structure of the titanium adhesion layer is the same as that of the interdigital platinum electrodes, and the gas sensitive film is the graphene, stannic oxide and zinc oxide ternary composite; the ternary composite is prepared by mixing graphene, stannic oxide and zinc oxide and is of a three-dimensional porous structure. Before and after the gas sensitive film makes contact with gas to be tested, the resistance of the gas sensitive film can change, and the sensitivity of the sensor can be obtained by measuring resistance changes between the interdigital platinum electrodes. The sensor has high response sensitivity, rapid response recovery rate and good response reversibility at room temperature, and the problem that the a stannic oxide and zinc oxide gas sensor can work only at high temperature is solved.
Description
Technical field
The invention belongs to gas sensor technical field, be specifically related to a kind of stone with room temperature air-sensitive response characteristic
Mertenyl resistor-type gas sensor and preparation method thereof, particularly relate to a kind of based on Graphene/tin ash/
The resistor-type gas sensor of zinc oxide composite, preparation method and applications.
Background technology
Along with industrial or agricultural and the fast development of transportation, problem of environmental pollution is more and more prominent.The nearest
Over Nian, toxic and harmful, the discharge capacity of flammable explosive gas increase day by day, the gas in environment is carried out accurately,
Continuous print detection becomes problem demanding prompt solution, this just application for gas sensor provide wide space.
Gas sensor is the chemical sensor that a class is important, industrial and agricultural production, process control, environmental monitoring and guarantor
Protect and have a wide range of applications with fields such as anti-terrorisms.Development has high sensitivity, low cost, low-power consumption, miniaturization
High performance gas sensor etc. advantage becomes the study hotspot of scientific research field and industrial circle.Wherein, sensitive material
The core of gas sensor, improve gas sensor performance it is crucial that exploitation has the gas of excellent response characteristic
Quick material.
At present, the conductor oxidate with tin ash, zinc oxide as representative becomes a most widely used class
Sensitive material, it has the advantages such as convenient, with low cost, the wide material sources of preparation, but there is also some not simultaneously
Foot, such as, less stable, affected relatively big by humidity, selectivity is not ideal enough.It is based particularly on metal
The gas sensor of oxide is required for working at a higher temperature, and this makes the power consumption of element bigger, it is difficult to
Prepare portable instrument.The highest operating temperature directly affects the stability of sensor, nor can be used for
Exist in the environment of flammable explosive gas so that it is application is subject to certain restrictions.
In order to solve this problem, the operating temperature of reduction sensor, the gas sensitive of exploitation working and room temperature are subject to
The extensive concern of researcher.The composite of metal-oxide and conducting polymer is prepared in researchers' trial, grinds
System can the gas sensor of working and room temperature.Although achieve room temperature detected gas, but metal-oxide and conduction
Polymer composites shows the problems such as sensitivity is low, response recovery is slow, seriously hinders it to apply further.
In recent years, the Two-dimensional Carbon based nano-material with Graphene as representative quickly grows, and becomes the focus of material circle research.
Conductivity at room temperature and fast carrier mobility that Graphene has are that the gas sensitive developing working and room temperature provides
New thinking.Research finds that grapheme material can realize room temperature detected gas really.Additionally, Graphene with
The compound sensitivity that can improve graphene-based gas sensor further of conductor oxidate, improves response extensive
Complex-velocity rate, is even expected to the highly sensitive gas detecting realizing under room temperature.Develop graphene-based room temperature air sensor
Become one of important directions of sensor field research, develop very fast.
Summary of the invention
It is an object of the invention to provide a kind of Graphene/bis-at room temperature with high sensitivity gas response characteristic
The resistor-type gas sensor of stannum oxide/zinc oxide composite, preparation method and applications.
A kind of resistor-type gas sensing based on Graphene/tin ash/zinc oxide composite of the present invention
Device, it is characterised in that: successively by monocrystalline substrate, silicon dioxide layer, titanium adhesion layer, interdigital platinum electrode,
The gas-sensitive film composition of silicon dioxide layer and the coating of interdigital platinum electrode surface；Titanium adhesion layer and interdigital platinum electrode
Structure identical, gas-sensitive film is Graphene/tin ash/zinc oxide trielement composite material；Gas sensitization
Before and after film contacts gas to be measured, its resistance can change, by measuring the change of resistance between interdigital platinum electrode,
The sensitivity of sensor can be obtained.
Described Graphene/tin ash/zinc oxide trielement composite material, by Graphene, tin ash and oxidation
Zinc mixes, and its mass ratio is 1:5～100:1～50, and trielement composite material is three-dimensional porous structure, hole
A size of 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, the thickness of the most interdigital platinum electrode of platinum metal layer is 50～200nm, and the logarithm of electrode is 4～6 right, electrode
Width be 50～100 μm, the spacing between electrode refers to is 50～100 μm, and connecting on interdigital platinum electrode has
Lead-in wire；The thickness of gas-sensitive film is 10～50 μm.
The system of Graphene/tin ash of the present invention/zinc oxide trielement composite material resistor-type gas sensor
Preparation Method, its step is as follows:
(1) with monocrystal silicon as substrate, using thermal oxidation method to prepare silicon dioxide layer at monocrystalline silicon surface, thickness is
150～300nm；Utilizing magnetron sputtering method at the surface titanium deposition adhesion layer of silicon dioxide, thickness is
40～90nm；Utilizing magnetron sputtering method to deposit platinum metal layer on titanium adhesion layer surface, thickness is
50～200nm；At platinum metal surface spin coating photoresist, thickness is 1～2 μm；Will be with interdigital platinum electricity
The photolithography plate that pole figure is identical is placed on photoresist surface, at the exposed under UV light 15 minutes of 350W,
Then developing with sodium hydroxide solution, the photoresist exposed after development is removed；Recycling argon from
Son bombardment platinum metal layer and titanium adhesion layer surface, be not photo-etched platinum metal layer and titanium adhesion layer that glue is covered
It is removed, then washes unexposed photoresist with ethanol solution, thus obtain interdigital electrode knot
The titanium adhesion layer of structure and interdigital platinum electrode, the logarithm of electrode is 4～6 right, and the width of electrode is 50～100
μm, the spacing between electrode refers to is 50～100 μm.
(2) prepare with ethanol, water successively ultrasonic cleaning surface and have the monocrystalline substrate of interdigital platinum electrode, dry；
(3) preparation graphene oxide water solution, the concentration of graphene oxide water solution is 0.1mg/mL～5
Mg/mL, is subsequently adding butter of tin, and ultrasonic disperse makes it mix fully, graphene oxide, tetrachloro
The quality amount ratio changing stannum and water is 1:10～200:5000～100000；Above-mentioned solution is existed
160～180 DEG C of Water Under thermal responses 12～24 hours, prepare Graphene/tin dioxide composite material
Solution, by composite solution centrifugation, washes and dries, it is thus achieved that Graphene/tin ash is multiple
Condensation material；Graphene/tin dioxide composite material is joined in methanol, Graphene and the matter of methanol
Amount amount ratio is 1:4000～200000；It is subsequently adding zinc nitrate and potassium hydroxide, Graphene, two
The weight ratio of stannum oxide, zinc nitrate and potassium hydroxide is 1:5～100:2～150:4～300, stirs
Mix and ultrasonic make it be uniformly dispersed；Above-mentioned solution is put in oil bath at 60～80 DEG C reaction 1～12
Hour, prepare Graphene/tin ash/zinc oxide trielement composite material solution；Above-mentioned solution is carried out
Centrifugation, wash and dry, it is thus achieved that Graphene/tin ash/zinc oxide trielement composite material.
(4) Graphene/tin ash/zinc oxide trielement composite material prepared by step (3) is distributed in water,
The concentration of composite aqueous solution is 1～10mg/mL；This solution is coated with step (2) obtain
The monocrystalline substrate surface with interdigital platinum electrode, then heat treatment 1～4 at 80～130 DEG C
Hour, the thickness of the sensitive thin film obtained is 10～50 μm, thus prepares based on Graphene/titanium dioxide
The resistor-type gas sensor of stannum/zinc oxide composite.
Gas sensor prepared by the present invention is used for NO2Room temperature response, the concentration of nitrogen dioxide is 1～100
Ppm, is preferably 1～5ppm.
The invention have the advantage that
1) between silicon dioxide and interdigital platinum electrode, add titanium adhesion layer, improve interdigital platinum electrode and silicon dioxide
The adhesive force of substrate, improves the stability of device.
2) tin ash and the introducing of zinc oxide in composite, can stop graphene sheet layer further
Reunite, be effectively improved the specific surface area of composite.Prepared Graphene/tin ash/zinc oxide is combined
Material has three-dimensional porous structure, big specific surface area so that sensor at room temperature has the highest response spirit
Sensitivity, quickly response regeneration rate and good response reversibility, solve tin ash and zinc oxide gas
Sensor typically requires the most workable problem.
3) using wet chemistry method to prepare Graphene/tin ash/zinc oxide composite, method is simple, it is easy to behaviour
Make, with low cost.And can be by controlling reaction temperature, response time and the ratio etc. of pre-reaction material
Experiment parameter realizes the regulation and control of the performances such as the composition of graphene-based composite, structure.
4) introducing of Graphene in composite, can significantly increase the electric conductivity of sensitive material, it is to avoid logical
Often tin ash and zinc oxide are because room temperature resistance is too high, and response sensitivity is extremely low and cannot realize room temperature detection gas
Body.
5) in composite tin ash and two kinds of Nanoparticle Modifieds of zinc oxide on the surface of Graphene, by
The surface activity site that tin ash is different with zinc oxide, it is achieved the regulation and control of double activated site, surface promote sensor
Sensitive property.
6) tin ash and the introducing of zinc oxide in composite, can form multiple heterojunction structure in the material
Including the heterojunction structure between Graphene and tin ash and zinc oxide semi-conductor, between tin ash and zinc oxide
Heterojunction structure, the semiconducting behavior of regulation and control Graphene and architectural feature, it is achieved the lifting of sensor performance.
7) use wet chemistry method at graphenic surface in-situ preparation tin ash and zinc oxide nano-particle, permissible
Significantly increase the combination of tin ash and zinc oxide and carbon-based material, improve the conductivity at room temperature of material, favorably
In realizing room temperature detected gas.The composite solution of preparation can use the methods such as spin coating to become in interdigital electrode
Film, it is easy to processing, can prepare gas sensor easily, solves traditional metal oxide gas sensing
Device needs high temperature sintering, the problem of processed complex.
Accompanying drawing explanation
Fig. 1 is the structural representation of the gas sensor of the present invention.
Wherein: monocrystal silicon 1, silicon dioxide layer 2, titanium adhesion layer 3, interdigital platinum electrode 4, gas-sensitive film
5, lead-in wire 6,7.
Fig. 2 is the X-ray diffraction spectrogram of Graphene/tin ash/zinc oxide composite.
Fig. 3 is that Graphene/tin ash/zinc oxide composite gas sensor is to 5ppm NO2Room temperature move
State response recovery curve.
Fig. 4 is that Graphene/tin ash/zinc oxide composite gas sensor is to 5ppm NO2Room temperature ring
(sensitivity definition is that sensor is in atmosphere with at NO to answer sensitivity2In gas, resistance between interdigital platinum electrode
Ratio) with gas concentration change curve.
Fig. 5 is that Graphene/tin ash/zinc oxide composite gas sensor is to 5ppm NO2Room temperature ring
The repeated curve answered.
Detailed description of the invention
The present invention is further illustrated below in conjunction with drawings and Examples.
Embodiment 1
(1) with monocrystal silicon as substrate, using thermal oxidation method to generate silicon dioxide layer at monocrystalline silicon surface, thickness is
150nm, utilizing magnetron sputtering method is 40 at the surface titanium deposition adhesion layer of silicon dioxide, thickness
nm；Utilizing magnetron sputtering method to deposit platinum metal layer on titanium adhesion layer surface, thickness is 50nm；?
Platinum metal surface spin coating BP212 (Kempur Microelectronic INC) positive photoresist, thickness
It it is 1 μm；The photolithography plate identical with interdigital platinum electrode figure is placed on photoresist surface, at 350W
Exposed under UV light 15 minutes, then show with the sodium hydroxide solution that mass fraction is 5/1000ths
Shadow, the photoresist exposed after development is removed；Recycling argon ion bombardment platinum metal layer and titanium stick
Attached layer surface, is not photo-etched platinum metal layer that glue covers and titanium adhesion layer is removed；Then ethanol is used
Solution washes unexposed photoresist, thus the titanium obtaining interdigital platinum electrode and interdigitated electrode structure sticks
Attached layer, the logarithm of interdigital platinum electrode is 4 right, and the width of electrode is 50 μm, electrode refer between spacing
It is 50 μm.
(2) being printed on the monocrystal silicon of interdigital platinum electrode with ethanol, water successively ultrasonic cleaning surface is substrate, dries stand-by；
(3) preparation 1mL concentration is the graphene oxide water solution of 0.1mg/mL, adds graphene oxide into
In aqueous solution, being subsequently adding butter of tin, ultrasonic disperse makes it mix fully, graphene oxide, four
The weight ratio of stannic chloride and water is 1:10:5000；By above-mentioned solution hydro-thermal reaction at 180 DEG C
24 hours, prepare Graphene/tin dioxide composite material solution, above-mentioned solution is centrifuged separate,
Washing and drying, it is thus achieved that Graphene/tin dioxide composite material；By Graphene/tin ash to methanol
In solution, Graphene is 1:4000 with the weight ratio of methanol；It is subsequently adding zinc nitrate and potassium hydroxide,
The weight ratio of Graphene, tin ash, zinc nitrate and potassium hydroxide is 1:5:2:4, stirring and
Ultrasonic it is made to be uniformly dispersed；Above-mentioned solution is put in oil bath at 60 DEG C reaction 12 hours, system
Obtain Graphene/tin ash/zinc oxide trielement composite material solution；Above-mentioned solution is centrifuged separate,
Washing and drying, it is thus achieved that Graphene/tin ash/zinc oxide trielement composite material.Above-mentioned solution is entered
Row centrifugation, wash, dry, it is thus achieved that Graphene/tin ash/zinc oxide trielement composite material,
Product quality is 240mg.
Graphene in obtained trielement composite material: tin ash: the part by weight of zinc oxide is 1:
5:1, trielement composite material is three-dimensional porous structure, and hole dimension is 3nm, and BET specific surface area is
100m2/g。
(4) Graphene/tin ash/zinc oxide trielement composite material prepared by step (3) is distributed in water,
Preparing the aqueous solution of Graphene/tin ash/zinc oxide trielement composite material, the concentration of composite is
1mg/mL；Above-mentioned solution is coated with the surface of silicon with interdigital platinum electrode of step (2),
At 80 DEG C, heat treatment obtains sensitive material film in 4 hours, and the thickness of thin film is 10 μm, prepares
Resistor-type gas sensor based on Graphene/tin ash/zinc oxide composite.
Embodiment 2
(1) with monocrystal silicon as substrate, using thermal oxidation method to generate silicon dioxide layer at monocrystalline silicon surface, thickness is
180nm, utilizing magnetron sputtering method is 60 at the surface titanium deposition adhesion layer of silicon dioxide, thickness
nm；Utilizing magnetron sputtering method to deposit platinum metal layer on titanium adhesion layer surface, thickness is 100nm；?
Platinum metal surface spin coating BP212 (Kempur Microelectronic INC) positive photoresist, thickness
It it is 1 μm；The photolithography plate identical with interdigital platinum electrode figure is placed on photoresist surface, at 350W
Exposed under UV light 15 minutes, then show with the sodium hydroxide solution that mass fraction is 5/1000ths
Shadow, the photoresist exposed after development is removed；Then recycling argon ion bombardment platinum metal layer and
Titanium adhesion layer surface, is not photo-etched platinum metal layer that glue covers and titanium adhesion layer is removed；Then use
Ethanol solution washes unexposed photoresist, thus obtains interdigital platinum electrode and interdigitated electrode structure
Titanium adhesion layer, it is thus achieved that interdigital platinum electrode, the logarithm of electrode is 4 right, and the width of electrode is 70 μm,
Spacing between electrode refers to is 50 μm.
(2) being printed on the monocrystal silicon of interdigital platinum electrode with ethanol, water successively ultrasonic cleaning surface is substrate, dries stand-by；
(3) preparation 1mL concentration is the graphene oxide water solution of 0.5mg/mL, adds graphene oxide into
In aqueous solution, being subsequently adding butter of tin, ultrasonic disperse makes it mix fully, graphene oxide, four
The weight ratio of stannic chloride and water is 1:50:1000；By above-mentioned solution hydro-thermal reaction at 160 DEG C
18 hours, prepare Graphene/tin dioxide composite material solution, above-mentioned solution is centrifuged separate,
Washing and drying, it is thus achieved that Graphene/tin dioxide composite material；By Graphene/tin ash to methanol
In solution, Graphene is 1:5000 with the weight ratio of methanol；It is subsequently adding zinc nitrate and potassium hydroxide,
The weight ratio of Graphene, tin ash, zinc nitrate and potassium hydroxide is 1:10:25:50, stirs
Mix and ultrasonic make it be uniformly dispersed；Above-mentioned solution is put in oil bath at 60 DEG C reaction 8 hours,
Prepare Graphene/tin ash/zinc oxide trielement composite material solution；Above-mentioned solution is centrifuged point
From, wash and dry, it is thus achieved that Graphene/tin ash/zinc oxide trielement composite material.By above-mentioned molten
Liquid is centrifuged separating, washes, dries, it is thus achieved that Graphene/tin ash/zinc oxide tri compound material
Material, product quality is 280mg.
Graphene in obtained trielement composite material: tin ash: the part by weight of zinc oxide is 1:
10:5, trielement composite material is three-dimensional porous structure, and hole dimension is 5nm, BET specific surface area
For 150m2/g。
(4) Graphene/tin ash/zinc oxide trielement composite material prepared by step (3) is distributed in water,
Preparing the aqueous solution of Graphene/tin ash/zinc oxide trielement composite material, the concentration of composite is
2mg/mL；Above-mentioned solution is coated with the surface of silicon with interdigital platinum electrode of step (2),
At 80 DEG C, heat treatment obtains sensitive material film in 2 hours, and the thickness of thin film is 20 μm, prepares
Resistor-type gas sensor based on Graphene/tin ash/zinc oxide composite.
Embodiment 3
(1) with monocrystal silicon as substrate, using thermal oxidation method to generate silicon dioxide layer at monocrystalline silicon surface, thickness is
210nm, utilizing magnetron sputtering method is 60 at the surface titanium deposition adhesion layer of silicon dioxide, thickness
nm；Utilizing magnetron sputtering method to deposit platinum metal layer on titanium adhesion layer surface, thickness is 100nm；?
Platinum metal surface spin coating BP212 (Kempur Microelectronic INC) positive photoresist, thickness
It it is 1 μm；The photolithography plate identical with interdigital platinum electrode figure is placed on photoresist surface, at 350W
Exposed under UV light 15 minutes, then show with the sodium hydroxide solution that mass fraction is 5/1000ths
Shadow, the photoresist exposed after development is removed；Then recycling argon ion bombardment platinum metal layer and
Titanium adhesion layer surface, is not photo-etched platinum metal layer that glue covers and titanium adhesion layer is removed；Then use
Ethanol solution washes unexposed photoresist, thus obtains interdigital platinum electrode and interdigitated electrode structure
Titanium adhesion layer, it is thus achieved that interdigital platinum electrode, the logarithm of electrode is 5 right, and the width of electrode is 70 μm,
Spacing between electrode refers to is 80 μm.
(2) being printed on the monocrystal silicon of interdigital platinum electrode with ethanol, water successively ultrasonic cleaning surface is substrate, dries stand-by；
(3) preparation 1mL concentration is the graphene oxide water solution of 1mg/mL, adds graphene oxide into
In aqueous solution, being subsequently adding butter of tin, ultrasonic disperse makes it mix fully, graphene oxide, four
The weight ratio of stannic chloride and water is 1:50:10000；On by, at 170 DEG C, hydro-thermal reaction 18 is little
Time, prepare Graphene/tin dioxide composite material solution, above-mentioned solution is centrifuged separation, water
Wash and dry, it is thus achieved that Graphene/tin dioxide composite material；Graphene/tin ash is molten to methanol
In liquid, Graphene is 1:10000 with the weight ratio of methanol；It is subsequently adding zinc nitrate and potassium hydroxide,
The weight ratio of Graphene, tin ash, zinc nitrate and potassium hydroxide is 1:25:50:100, stirs
Mix and ultrasonic make it be uniformly dispersed；Above-mentioned solution is put in oil bath at 70 DEG C reaction 12 hours,
Prepare Graphene/tin ash/zinc oxide trielement composite material solution；Above-mentioned solution is centrifuged point
From, wash and dry, it is thus achieved that Graphene/tin ash/zinc oxide trielement composite material.By above-mentioned molten
Liquid is centrifuged separating, washes, dries, it is thus achieved that Graphene/tin ash/zinc oxide tri compound material
Material, product quality is 300mg.
Graphene in obtained trielement composite material: tin ash: the part by weight of zinc oxide is 1:
25:10, trielement composite material is three-dimensional porous structure, and hole dimension is 7nm, BET specific surface area
For 180m2/g。
(4) Graphene/tin ash/zinc oxide trielement composite material prepared by step (3) is distributed in water,
Preparing the aqueous solution of Graphene/tin ash/zinc oxide trielement composite material, the concentration of composite is
4mg/mL；Above-mentioned solution is coated with the surface of silicon with interdigital platinum electrode of step (2),
At 90 DEG C, heat treatment obtains sensitive material film in 4 hours, and the thickness of thin film is 30 μm, prepares
Resistor-type gas sensor based on Graphene/tin ash/zinc oxide composite.
Embodiment 4
(1) with monocrystal silicon as substrate, using thermal oxidation method to generate silicon dioxide layer at monocrystalline silicon surface, thickness is
240nm, utilizing magnetron sputtering method is 80 at the surface titanium deposition adhesion layer of silicon dioxide, thickness
nm；Utilizing magnetron sputtering method to deposit platinum metal layer on titanium adhesion layer surface, thickness is 150nm；?
Platinum metal surface spin coating BP212 (Kempur Microelectronic INC) positive photoresist, thickness
It is 2 μm；The photolithography plate identical with interdigital platinum electrode figure is placed on photoresist surface, at 350W
Exposed under UV light 15 minutes, then show with the sodium hydroxide solution that mass fraction is 5/1000ths
Shadow, the photoresist exposed after development is removed；Then recycling argon ion bombardment platinum metal layer and
Titanium adhesion layer surface, is not photo-etched platinum metal layer that glue covers and titanium adhesion layer is removed；Then use
Ethanol solution washes unexposed photoresist, thus obtains interdigital platinum electrode and interdigitated electrode structure
Titanium adhesion layer, it is thus achieved that interdigital platinum electrode, the logarithm of electrode is 5 right, and the width of electrode is 80 μm,
Spacing between electrode refers to is 80 μm.
(2) being printed on the monocrystal silicon of interdigital platinum electrode with ethanol, water successively ultrasonic cleaning surface is substrate, dries stand-by；
(3) preparation 1mL concentration is the graphene oxide water solution of 1.5mg/mL, adds graphene oxide into
In aqueous solution, being subsequently adding butter of tin, ultrasonic disperse makes it mix fully, graphene oxide, four
The weight ratio of stannic chloride and water is 1:100:50000；By anti-for above-mentioned solution hydro-thermal at 170 DEG C
Answer 16 hours, prepare Graphene/tin dioxide composite material solution, above-mentioned solution is centrifuged point
From, wash and dry, it is thus achieved that Graphene/tin dioxide composite material；Graphene/tin ash is arrived
In methanol solution, Graphene is 1:50000 with the weight ratio of methanol；It is subsequently adding zinc nitrate and hydrogen
Potassium oxide, the weight ratio of Graphene, tin ash, zinc nitrate and potassium hydroxide is 1:50:75:
150, stirring and ultrasonic make it be uniformly dispersed；Above-mentioned solution is put in oil bath at 70 DEG C reaction 8
Hour, prepare Graphene/tin ash/zinc oxide trielement composite material solution；Above-mentioned solution is carried out
Centrifugation, wash and dry, it is thus achieved that Graphene/tin ash/zinc oxide trielement composite material.Will
Above-mentioned solution is centrifuged separating, washes, dries, it is thus achieved that Graphene/tin ash/zinc oxide ternary
Composite, product quality is 320mg.
Graphene in obtained trielement composite material: tin ash: the part by weight of zinc oxide is 1:
50:15, trielement composite material is three-dimensional porous structure, and hole dimension is 8nm, BET specific surface area
For 200m2/g。
(4) Graphene/tin ash/zinc oxide trielement composite material prepared by step (3) is distributed in water,
Preparing the aqueous solution of Graphene/tin ash/zinc oxide trielement composite material, the concentration of composite is
6mg/mL；Above-mentioned solution is coated with the surface of silicon with interdigital platinum electrode of step (2),
At 100 DEG C, heat treatment obtains sensitive material film in 3 hours, and the thickness of thin film is 30 μm, system
Must be based on the resistor-type gas sensor of Graphene/tin ash/zinc oxide composite.
Embodiment 5
(1) with monocrystal silicon as substrate, using thermal oxidation method to generate silicon dioxide layer at monocrystalline silicon surface, thickness is
270nm, utilizing magnetron sputtering method is 80 at the surface titanium deposition adhesion layer of silicon dioxide, thickness
nm；Utilizing magnetron sputtering method to deposit platinum metal layer on titanium adhesion layer surface, thickness is 150nm；?
Platinum metal surface spin coating BP212 (Kempur Microelectronic INC) positive photoresist, thickness
It is 2 μm；The photolithography plate identical with interdigital platinum electrode figure is placed on photoresist surface, at 350W
Exposed under UV light 15 minutes, then show with the sodium hydroxide solution that mass fraction is 5/1000ths
Shadow, the photoresist exposed after development is removed；Then recycling argon ion bombardment platinum metal layer and
Titanium adhesion layer surface, is not photo-etched platinum metal layer that glue covers and titanium adhesion layer is removed；Then use
Ethanol solution washes unexposed photoresist, thus obtains interdigital platinum electrode and interdigitated electrode structure
Titanium adhesion layer, it is thus achieved that interdigital platinum electrode, the logarithm of electrode is 5 right, and the width of electrode is 90 μm,
Spacing between electrode refers to is 100 μm.
(2) being printed on the monocrystal silicon of interdigital platinum electrode with ethanol, water successively ultrasonic cleaning surface is substrate, dries stand-by；
(3) preparation 1mL concentration is the graphene oxide water solution of 3mg/mL, adds graphene oxide into
In aqueous solution, being subsequently adding butter of tin, ultrasonic disperse makes it mix fully, graphene oxide, four
The weight ratio of stannic chloride and water is 1:100:50000；By anti-for above-mentioned solution hydro-thermal at 180 DEG C
Answer 16 hours, prepare Graphene/tin dioxide composite material solution, above-mentioned solution is centrifuged point
From, wash and dry, it is thus achieved that Graphene/tin dioxide composite material；Graphene/tin ash is arrived
In methanol solution, Graphene is 1:100000 with the weight ratio of methanol；Be subsequently adding zinc nitrate and
Potassium hydroxide, the weight ratio of Graphene, tin ash, zinc nitrate and potassium hydroxide is 1:75:100:
200, stirring and ultrasonic make it be uniformly dispersed；Above-mentioned solution is put in oil bath at 80 DEG C reaction 8
Hour, prepare Graphene/tin ash/zinc oxide trielement composite material solution；Above-mentioned solution is carried out
Centrifugation, wash and dry, it is thus achieved that Graphene/tin ash/zinc oxide trielement composite material.Will
Above-mentioned solution is centrifuged separating, washes, dries, it is thus achieved that Graphene/tin ash/zinc oxide ternary
Composite, product quality is 340mg.
Graphene in obtained trielement composite material: tin ash: the part by weight of zinc oxide is 1:
75:25, trielement composite material is three-dimensional porous structure, and hole dimension is 10nm, BET specific surface
Amass as 210m2/g。
(4) Graphene/tin ash/zinc oxide trielement composite material prepared by step (3) is distributed in water,
Preparing the aqueous solution of Graphene/tin ash/zinc oxide trielement composite material, the concentration of composite is
8mg/mL；Above-mentioned solution is coated with the surface of silicon with interdigital platinum electrode of step (2),
At 110 DEG C, heat treatment obtains sensitive material film in 2 hours, and the thickness of thin film is 40 μm, system
Must be based on the resistor-type gas sensor of Graphene/tin ash/zinc oxide composite.
Embodiment 6
(1) with monocrystal silicon as substrate, using thermal oxidation method to generate silicon dioxide layer at monocrystalline silicon surface, thickness is
300nm, utilizing magnetron sputtering method is 90 at the surface titanium deposition adhesion layer of silicon dioxide, thickness
nm；Utilizing magnetron sputtering method to deposit platinum metal layer on titanium adhesion layer surface, thickness is 200nm；?
Platinum metal surface spin coating BP212 (Kempur Microelectronic INC) positive photoresist, thickness
It is 2 μm；The photolithography plate identical with interdigital platinum electrode figure is placed on photoresist surface, at 350W
Exposed under UV light 15 minutes, then show with the sodium hydroxide solution that mass fraction is 5/1000ths
Shadow, the photoresist exposed after development is removed；Then recycling argon ion bombardment platinum metal layer and
Titanium adhesion layer surface, is not photo-etched platinum metal layer that glue covers and titanium adhesion layer is removed；Then use
Ethanol solution washes unexposed photoresist, thus obtains interdigital platinum electrode and interdigitated electrode structure
Titanium adhesion layer, it is thus achieved that interdigital platinum electrode, the logarithm of electrode is 6 right, and the width of electrode is 90 μm,
Spacing between electrode refers to is 100 μm.
(2) being printed on the monocrystal silicon of interdigital platinum electrode with ethanol, water successively ultrasonic cleaning surface is substrate, dries stand-by；
(3) preparation 1mL concentration is the graphene oxide water solution of 5mg/mL, adds graphene oxide into
In aqueous solution, being subsequently adding butter of tin, ultrasonic disperse makes it mix fully, graphene oxide, four
The weight ratio of stannic chloride and water is 1:200:100000；By anti-for above-mentioned solution hydro-thermal at 180 DEG C
Answer 12 hours, prepare Graphene/tin dioxide composite material solution, above-mentioned solution is centrifuged point
From, wash and dry, it is thus achieved that Graphene/tin dioxide composite material；Graphene/tin ash is arrived
In methanol solution, Graphene is 1:200000 with the weight ratio of methanol；Be subsequently adding zinc nitrate and
Potassium hydroxide, the weight ratio of Graphene, tin ash, zinc nitrate and potassium hydroxide is 1:100:
150:300, stirring and ultrasonic make it be uniformly dispersed；Above-mentioned solution is put in oil bath at 80 DEG C
React 1 hour, prepare Graphene/tin ash/zinc oxide trielement composite material solution；By above-mentioned molten
Liquid is centrifuged separating, washing and dry, it is thus achieved that Graphene/tin ash/zinc oxide tri compound material
Material.It is centrifuged above-mentioned solution separating, washes, dries, it is thus achieved that Graphene/tin ash/oxidation
Zinc trielement composite material, product quality is 360mg.
Graphene in obtained trielement composite material: tin ash: the part by weight of zinc oxide is 1:
100:50, trielement composite material is three-dimensional porous structure, and hole dimension is 10nm, BET specific surface
Amass as 230m2/g。
(4) Graphene/tin ash/zinc oxide trielement composite material prepared by step (3) is distributed in water,
Preparing the aqueous solution of Graphene/tin ash/zinc oxide trielement composite material, the concentration of composite is
10mg/mL；Above-mentioned solution is coated with the surface of silicon with interdigital platinum electrode of step (2),
At 130 DEG C, heat treatment obtains sensitive material film in 1 hour, and the thickness of thin film is 50 μm, system
Must be based on the resistor-type gas sensor of Graphene/tin ash/zinc oxide composite.
Graphene/tin ash/zinc oxide trielement composite material X-ray diffraction the spectrogram such as figure of embodiment 1 preparation
Shown in 2, as seen from Figure 2, composite has the diffraction typically belonging to tin ash and zinc oxide
Peak, illustrates that composite contains by tin ash and two kinds of metal-oxides of oxidisability.
The gas sensor based on Graphene/tin ash/zinc oxide trielement composite material of embodiment 1 preparation exists
Under room temperature, the response recovery curve to variable concentrations nitrogen dioxide is shown in Fig. 3.It can be seen that preparation is graphene-based
Gas sensor has response the highest, quickly to the nitrogen dioxide of variable concentrations, and response time is less than 1 minute,
And sensor has good reversibility.
The gas sensor pair based on Graphene/tin ash/zinc oxide trielement composite material of embodiment 1 preparation
The response sensitivity curve of variable concentrations nitrogen dioxide is shown in Fig. 4.It can be seen that sensor is at room temperature to low dense
The nitrogen dioxide of degree has higher sensitivity, reaches 1.5 for 1ppm nitrogen dioxide.
The gas sensor based on Graphene/tin ash/zinc oxide trielement composite material of embodiment 1 preparation exists
Under room temperature, the response repeatability curve to 5ppm nitrogen dioxide is shown in Fig. 5.It can be seen that at room temperature through two
The multiple loop test of nitrogen oxide-air, its response curve is almost unchanged, shows that this sensor has good sound
Should repeatability.
Claims (6)
1. a resistor-type gas sensor based on Graphene/tin ash/zinc oxide composite, its feature exists
In: successively by monocrystalline substrate, silicon dioxide layer, titanium adhesion layer, interdigital platinum electrode, at silicon dioxide
The gas-sensitive film composition of layer and the coating of interdigital platinum electrode surface；Titanium adhesion layer and the knot of interdigital platinum electrode
Structure is identical, and gas-sensitive film is Graphene/tin ash/zinc oxide trielement composite material；This ternary is multiple
Condensation material is mixed by Graphene, tin ash and zinc oxide, and its mass ratio is 1:5～100:1～50,
Trielement composite material is three-dimensional porous structure, and hole dimension is 3～10nm, and BET specific surface area is
100～230m2/g。
A kind of resistor-type gas based on Graphene/tin ash/zinc oxide composite
Body sensor, it is characterised in that: the thickness of silicon dioxide layer is 150～300nm, the thickness of titanium adhesion layer
Degree is 40～90nm, and the thickness of the most interdigital platinum electrode of platinum metal layer is 50～200nm, the logarithm of electrode
Being 4～6 right, the width of electrode is 50～100 μm, and the spacing between electrode refers to is 50～100 μm, gas
The thickness of body sensitive thin film is 10～50 μm.
3. a kind of based on Graphene/tin ash/zinc oxide composite the resistor-type gas described in claim 1
The preparation method of sensor, its step is as follows:
(1) with monocrystal silicon as substrate, thermal oxidation method is used to prepare silicon dioxide layer at monocrystalline silicon surface；Utilize
Magnetron sputtering method is at the surface titanium deposition adhesion layer of silicon dioxide；Magnetron sputtering method is utilized to stick at titanium
Attached layer surface deposition platinum metal layer；At platinum metal surface spin coating photoresist, thickness is 1～2 μm；
The photolithography plate identical with interdigital platinum electrode figure is placed on photoresist surface, exposed under UV light,
Then developing with sodium hydroxide solution, the photoresist exposed after development is removed；Recycling
Argon ion bombardment platinum metal layer and titanium adhesion layer surface, be not photo-etched platinum metal layer that glue covers and
Titanium adhesion layer is removed, and then washes unexposed photoresist with ethanol solution, thus obtains
Obtain the titanium adhesion layer of interdigitated electrode structure and interdigital platinum electrode；
(2) prepare with ethanol, water successively ultrasonic cleaning surface and have the monocrystalline substrate of interdigital platinum electrode, dry；
(3) preparation graphene oxide water solution, the concentration of graphene oxide water solution is 0.1mg/mL～5
Mg/mL, is subsequently adding butter of tin, and ultrasonic disperse makes it mix fully, graphene oxide,
The quality amount ratio of butter of tin and water is 1:10～200:5000～100000；By above-mentioned molten
Liquid, 160～180 DEG C of Water Under thermal responses 12～24 hours, prepares Graphene/tin ash
Composite solution, by composite solution centrifugation, washes and dries, it is thus achieved that Graphene
/ tin dioxide composite material；Graphene/tin dioxide composite material is joined in methanol, stone
Ink alkene is 1:4000～200000 with the quality amount ratio of methanol；It is subsequently adding zinc nitrate and hydrogen
Potassium oxide, the weight ratio of Graphene, tin ash, zinc nitrate and potassium hydroxide is 1:5～100:
2～150:4～300, stirring and ultrasonic make it be uniformly dispersed；Above-mentioned solution is put in oil bath
React 1～12 hour at 60～80 DEG C, prepare Graphene/tin ash/zinc oxide ternary multiple
Condensation material solution；It is centrifuged above-mentioned solution separating, washing and dry, it is thus achieved that Graphene/
Tin ash/zinc oxide trielement composite material；
(4) Graphene/tin ash/zinc oxide trielement composite material prepared by step (3) is distributed in water,
The concentration of composite aqueous solution is 1～10mg/mL；This solution is coated with step (2)
The monocrystalline substrate surface with interdigital platinum electrode obtained, then at 80～130 DEG C at heat
Manage 1～4 hour, thus prepare resistance based on Graphene/tin ash/zinc oxide composite
Type gas sensor.
4. a kind of based on Graphene/tin ash/zinc oxide composite the resistor-type described in claim 1 or 2
Gas sensor is at detection NO2In application.
A kind of resistor-type gas based on Graphene/tin ash/zinc oxide composite
Body sensor is at detection NO2In application, it is characterised in that: NO2Concentration be 1～100ppm.
A kind of resistor-type gas based on Graphene/tin ash/zinc oxide composite
Body sensor is at detection NO2In application, it is characterised in that: NO2Concentration be 1～5ppm.
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