CN106990142A - A kind of NO based on graphene/tin dioxide quantal-point composite2Sensor and preparation method thereof - Google Patents

A kind of NO based on graphene/tin dioxide quantal-point composite2Sensor and preparation method thereof Download PDF

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Publication number
CN106990142A
CN106990142A CN201710319671.8A CN201710319671A CN106990142A CN 106990142 A CN106990142 A CN 106990142A CN 201710319671 A CN201710319671 A CN 201710319671A CN 106990142 A CN106990142 A CN 106990142A
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sensor
graphene
tin dioxide
earthenware
point composite
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王振宇
王延林
李秋霖
贾子光
孙伟
孙家斌
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Dalian University of Technology
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Dalian University of Technology
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/12Investigating 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
    • G01N27/125Composition of the body, e.g. the composition of its sensitive layer

Abstract

A kind of NO based on graphene/tin dioxide quantal-point composite2Sensor and preparation method thereof, belongs to gas sensor technical field.Described NO2Sensor is heater-type structure, including nickel-cadmium heating coil, Al2O3Earthenware, sensitive layer, Pt wires and two gold electrodes, nickel-cadmium heating coil are located at Al2O3The inside of earthenware, for heating NO2Sensor;Two gold electrodes are located at Al2O3The surface of earthenware, each gold electrode is connected with Pt wires, and measurement NO is realized by measuring the D.C. resistance resistance in different atmosphere between two gold electrodes2The function of concentration;Sensitive layer is wrapped in Al2O3On the outside of earthenware, and two gold electrodes are completely covered.The present invention makes sensitive material have high-specific surface area and dimensional effect concurrently using the cooperative effect of composite, prepares high-performance NO2Sensor;By changing the ratio of graphene and tin dioxide quantal-point, the sensitivity characteristic of sensor can be regulated and controled;Sensor prepared by the present invention has a good application prospect in terms of environmental monitoring.

Description

A kind of NO based on graphene/tin dioxide quantal-point composite2Sensor and its Preparation method
Technical field
The invention belongs to gas sensor domain, and in particular to one kind is based on graphene/tin dioxide quantal-point composite wood Resistance sensor of material and preparation method thereof, according to graphene/tin dioxide quantal-point composite sensitive membrane in work temperature Resistance variations under degree are realized to NO2Detection.
Background technology
NO2It is a kind of common dusty gas, it has strong impulse smell, harm is serious, is natural environment and people The dual killer of class health.Nitrogen dioxide can cause a variety of environmental problems interior on a large scale, and it forms photochemical fog One of principal element, is also one of source of acid rain.Photochemical fog can seriously damage the health of humans and animals, influence crop Growth, destroys construction material, influences atmospheric visibility.And acid rain can change the pH value of soil, the growth of crops is hindered, is caused The agriculture underproduction is even had no harvest;Forest cover can be destroyed, tree death is caused;Building and industrial equipment can be corroded, shortening it makes Use the life-span;Meeting polluted source, causes water body pH reductions, and significant damage is caused to fishery and Drinking Water for Residents safety is threatened.Two After nitrogen oxide is sucked by human body, strong impulse effect and corrosiveness can be produced to lung tissue, so as to cause pulmonary edema.Exhale Desorption system has the people such as asthmatics of illness, is easier to be influenceed by nitrogen dioxide.For children, nitrogen dioxide may Cause lung's maldevelopment.Research points out that long-term people's nitrogen dioxide of inhaling can cause lung's structural change.
In order to reduce or eliminate NO2Harm it will be controlled to discharge, thus to NO2Real-time and monitor just Seem very necessary.Current NO2The conventional method of detection mainly has Saltzman methods, chemoluminescence method and spectroscopic methodology etc..On The method of stating has Monitoring lower-cut low, the features such as sensitivity is high, but is due to that they generally require complex, expensive equipment, Be not suitable for carrying out real-time continuous monitoring to environmental gas.Therefore people place hope on comes to NO using gas sensor2Supervised Survey.According to national standard, NO2Annual, 24 hourly averages and 1 hour average concentration limit value are respectively 19.48ppb, 38.96ppb and 97.40ppb.Therefore, the NO applied to environmental monitoring2Sensor must have higher sensitivity with it is relatively low Monitoring lower-cut, in addition, in order to realize real-time online measuring, it should also have shorter response recovery time.
The content of the invention
The purpose of the present invention is to develop one kind to have the graphite of high sensitivity, low-detection lower limit and the extensive characteristic of quick response Alkene/tin dioxide quantal-point composite material base NO2Sensor.
In order to achieve the above object, the technical scheme is that:
A kind of NO based on graphene/tin dioxide quantal-point composite2Sensor, described NO2Sensor is indirect heat Formula structure, including nickel-cadmium heating coil, Al2O3Earthenware, sensitive layer, Pt wires and two gold electrodes, its structure such as Fig. 1 It is shown.Described nickel-cadmium heating coil is located at Al2O3The inside of earthenware, for heating NO2Sensor;Two gold electrodes Positioned at Al2O3The surface of earthenware, each gold electrode is connected with Pt wires, by measuring two gold electrodes in different atmosphere Between D.C. resistance resistance realize measurement NO2The function of concentration;Sensitive layer is wrapped in Al2O3On the outside of earthenware, and it is completely covered two Bar gold electrode.
Described sensitive layer is graphene/tin dioxide quantal-point composite, and thickness is 15~30um.Described Al2O3 Earthenware is insulating barrier, and its internal diameter is 0.7~0.9mm, and external diameter is 1.0~1.5mm, and length is 4~5mm.Described single gold The width of electrode is 0.4~0.5mm, and the spacing of two gold electrodes is 0.5~0.6mm.The platinum filament drawn on described gold electrode Conductor length is 4~6mm, and platinum filament wire is by Al2O3Earthenware is welded on general heater-type hexagonal base and is capped protective cover. The number of turn of described nickel-cadmium heating coil is that 50~60 circles, resistance value are 30~40 Ω.
A kind of NO based on graphene/tin dioxide quantal-point composite2The preparation method of sensor, including following step Suddenly:
(1) graphene/tin dioxide quantal-point composite and ethanol are pressed 0.1~0.3:1 mass ratio is well mixed, Form slurry;Slurry is coated uniformly on Al of the surface with a pair of test gold electrodes2O3On the surface of earthenware, make its complete Cover gold electrode.
The coating thickness of described graphene/tin dioxide quantal-point composite is 15~30um, and graphene is in graphite Mass fraction in alkene/tin dioxide quantal-point composite is 1%-10%.Al2O3The internal diameter of earthenware is 0.7~0.9mm, External diameter is 1.0~1.5mm, and length is 4~5mm;The width of single gold electrode is 0.4~0.5mm, and the spacing of two gold electrodes is 0.5~0.6mm;The platinum filament wire drawn on gold electrode, its length is 4~6mm.
(2) Al of graphene/tin dioxide quantal-point composite will have been coated2O3Earthenware is placed and dried at room temperature Afterwards, it is transferred into 80 DEG C of baking ovens and continues to dry 30~60min.Nickel-cadmium heating coil is penetrated into Al2O3Earthenware is to it Heated, by the operating current size control NO for adjusting heater strip2The operating temperature of sensor, wherein nickel-cadmium are heated The number of turn of coil is that 50~60 circles, resistance value are 30~40 Ω.Finally by platinum filament wire by Al2O3Earthenware is welded on general On heater-type hexagonal base and it is capped protective cover;
(3) by Al2O3Sensor is positioned over aging 5-15 days in 200~400 DEG C of air ambients, obtains graphene/titanium dioxide Tin quantum dot composite material base NO2Gas sensor.
Graphene used in the present invention/tin dioxide quantal-point composite and preparation method thereof is:First, room temperature Under, it is 1 in mass ratio by graphene oxide and butter of tin:10~200 dissolve in deionized water, well mixed to obtain mixing molten Liquid.Secondly, at room temperature, hydrazine hydrate is added in mixed solution, dispersion liquid is obtained after stirring, wherein, graphene oxide with The mass ratio of hydrazine hydrate is 1:20-100.Finally, dispersion liquid is subjected to microwave hydrothermal reaction, product is obtained after cleaning, wherein, it is micro- Ripple hydrothermal temperature is 120-180 DEG C, and the reaction time is 5-120 minutes.Graphene/tin dioxide quantal-point composite In, tin dioxide quantal-point size uniformity, and it is evenly distributed on the both sides of graphene film.
The present invention operation principle be:
As graphene/tin dioxide quantal-point composite material base NO2When gas sensor is placed in air, the oxygen in air Qi leel can capture electronics in sensitive material adsorption, and from sensitive material, then with O2 -、O-Or O2-Etc. chemisorbed shape The form of state is present, while material surface will form depletion layer.At a suitable temperature, when sensor contacts to NO2During gas, NO2Gas molecule will be adsorbed in sensor surface.Due to NO2It is a kind of typical oxidizing gas, it has larger electronics parent And gesture, therefore, NO2Gas molecule can obtain electronics from sensitive material and be transformed into anion absorption, and this process will make quick Feel electron concentration in material to decline, resistance rise.We define sensitivity S=R of sensor hereing/Ra, wherein RaTo pass The aerial resistance value of sensor, RgIt is sensor in certain density NO2Resistance in atmosphere.For sensor response when Between be defined as after device is placed under test gas, the change of its resistance reaches to be hindered in resistance stable under test gas and air Value difference value 90% when required time, be defined as recovery time after device is transferred in air from tested gas, The change of its resistance reaches the time required during 90% of resistance difference in resistance stable in the air and under test gas.
Beneficial effects of the present invention are:
(1) from sensitive material selected angle:The present invention is cleverly designed to the sensitive material of sensor, by introducing High conductivity, the grapheme material of high-specific surface area improves the electrical properties of sensitive material, enhancing sensitive material and gas to be measured The contact of body, is conducive to the diffusion of gas molecule to improve the performance of sensor.And tin dioxide quantal-point due to size compared with Small, reactivity is higher, and can embody obvious dimensional effect, therefore it can reveal obvious response to gas meter to be measured. Therefore, high performance NO can be prepared by designing graphene/tin dioxide quantal-point composite2Sensor.
(2) senor operating temperature of exploitation is low, and response resume speed is fast, and Monitoring lower-cut is relatively low, reproducible.
(3) graphene/tin dioxide quantal-point composite material base NO that the present invention makes2The letter of gas sensor manufacture craft It is single, it is with low cost, it is adapted to industrial batch production.Had a good application prospect in terms of environmental monitoring.
(4) sensitivity characteristic of sensor can be regulated and controled by adjusting the mass fraction of graphene in composite, such as worked Temperature, response recovery time, sensitivity etc., this provides convenience for the expansion of sensor application environment.
Brief description of the drawings
Fig. 1 is graphene/tin dioxide quantal-point composite material base NO of the invention2The schematic diagram of sensor.
Fig. 2 is graphene/tin dioxide quantal-point composite material base NO same as Example 1 when being operated in 75 DEG C2Pass Sensor is in 50~150ppb NO2Response recovery curve in atmosphere.
Fig. 3 is graphene/tin dioxide quantal-point composite material base NO same as Example 1 when being operated in 75 DEG C2Pass Sensor is in 200~350ppb NO2Response recovery curve in atmosphere.
Fig. 4 is graphene/tin dioxide quantal-point composite material base NO same as Example 1 when being operated in 75 DEG C2Pass Sensor is in 350ppb NO2Response recovery curve in atmosphere.
Fig. 5 is graphene/tin dioxide quantal-point composite material base NO same as Example 1 when being operated in 75 DEG C2Pass Sensor sensitivity and NO2Relation between concentration.
In figure:1 nickel-cadmium heating coil;2Al2O3Earthenware;3 sensitive layers;4Pt wires;5 gold electrodes.
Embodiment
It is further to the present invention below in conjunction with the accompanying drawings to be stated, this hair can be better understood from according to following examples It is bright.
A kind of NO based on graphene/tin dioxide quantal-point composite2Sensor, described NO2Sensor is indirect heat Formula structure, including nickel-cadmium heating coil 1, Al2O3Earthenware 2, sensitive layer 3, Pt wires 4 and two gold electrodes 5, its structure As shown in Figure 1.Described nickel-cadmium heating coil 1 is located at Al2O3The inside of earthenware 2, for heating NO2Sensor;Two Gold electrode 5 is located at Al2O3The surface of earthenware 2, each gold electrode 5 is connected with Pt wires 4, by measuring in different atmosphere D.C. resistance resistance between two gold electrodes 5 realizes measurement NO2The function of concentration;Sensitive layer is wrapped in Al2O3The outside of earthenware 2, And two gold electrodes 5 are completely covered.
Fig. 2 is the identical graphene of embodiment 1/tin dioxide quantal-point composite material base NO when being operated in 75 DEG C2Sensing Device is in 50~150ppb NO2Response recovery curve in atmosphere.As can be seen that in atmosphere when, resistance is basically unchanged.Work as biography Sensor is placed in NO2When in atmosphere, sensor resistance gradually rises, and finally tends towards stability.Gas in sensor test environment Body is by NO2When being changed into air, resistance is gradually reduced, and is finally tended towards stability.In addition, with NO2The increase of concentration, it is observed that Sensor resistance change is more and more obvious.Fig. 3 is the identical graphene of embodiment 1/tin dioxide quantal-point when being operated in 75 DEG C Composite material base NO2Sensor is in 200~350ppb NO2Response recovery curve in atmosphere.As can be seen that in atmosphere when, Resistance is basically unchanged.When sensor is placed in NO2When in atmosphere, sensor resistance gradually rises, and finally tends towards stability.Work as sensing Gas in device test environment is by NO2When being changed into air, resistance is gradually reduced, and is finally tended towards stability.In addition, with NO2Concentration Increase, it is observed that sensor resistance change is more and more obvious.Fig. 4 is the identical graphite of embodiment 1 when being operated in 75 DEG C Alkene/tin dioxide quantal-point composite material base NO2Sensor is in 350ppb NO2Response recovery curve in atmosphere.As can be seen that The response resume speed of sensor is very fast, and its response time is about 6.5 minutes, and recovery time is about 1 minute.Fig. 5 is to be operated in At 75 DEG C, the identical graphene of embodiment 1/tin dioxide quantal-point composite material base NO2The sensitivity of sensor and NO2Concentration Between relation.As can be seen that with NO2The rise of concentration, sensitivity increase.Sensor is to 350ppb NO2Sensitivity be 227, to 50ppb NO2Sensitivity be 2.6, sensor has higher sensitivity and very low Monitoring lower-cut.
Embodiment 1
(1) graphene/tin dioxide quantal-point composite 0.2g and 2g ethanol that graphene mass fraction is about 2% are taken It is uniformly mixed to form slurry;The slurry is coated uniformly on Al of the surface with a pair of test gold electrodes2O3The surface of earthenware On, make it that gold electrode is completely covered.Wherein the thickness of graphene/tin dioxide quantal-point composite is 15~30um;Al2O3 The internal diameter of earthenware is 0.8mm, and external diameter is 1.2mm, and length is 5mm;The width of single gold electrode is 0.5mm, two gold electrodes Spacing be 0.5mm;The platinum filament wire drawn on gold electrode, its length is 5mm.
(2) earthenware for having coated graphene/tin dioxide quantal-point sensitive material is dried at room temperature for, then by it It is transferred in 80 DEG C of baking ovens and continues to dry 30min.Next nickel-cadmium heating coil is penetrated into Al2O3Earthenware comes to device Heated, the circle of the operating temperature of sensor, wherein heating coil is regulated and controled by adjusting the operating current size of heater strip Number is that 55 circles, resistance value are 40 Ω.Earthenware is welded on general heater-type hexagonal base and added finally by platinum filament wire Lid protective cover.
(3) finally by sensor in about 200 DEG C of air ambients aging 7 days, so as to obtain graphene/tin ash quantum Point composite material base NO2Gas sensor.
(4) static test system is utilized, sensor is tested at 75 DEG C to 50ppb NO2Response:Sensor is placed in In air atmosphere, sensor heating-up temperature is 75 DEG C;After after sensor resistance stabilization, it is 50ppb's that sensor is placed in into concentration NO2In atmosphere, again wait for sensor resistance and tend towards stability;After the resistance of sensor tends towards stability again, sensor is put In air atmosphere, sensor resistance is waited to return to initial value.
Embodiment 2
(1) graphene/tin dioxide quantal-point composite 0.2g and 2g ethanol that graphene mass fraction is about 2% are taken It is uniformly mixed to form slurry;The slurry is coated uniformly on Al of the surface with a pair of test gold electrodes2O3The surface of earthenware On, make it that gold electrode is completely covered.Wherein the thickness of graphene/tin dioxide quantal-point composite is 15~30um;Al2O3 The internal diameter of earthenware is 0.8mm, and external diameter is 1.2mm, and length is 5mm;The width of single gold electrode is 0.5mm, two gold electrodes Spacing be 0.5mm;The platinum filament wire drawn on gold electrode, its length is 5mm.
(2) earthenware for having coated graphene/tin dioxide quantal-point sensitive material is dried at room temperature for, then by it It is transferred in 80 DEG C of baking ovens and continues to dry 30min.Next nickel-cadmium heating coil is penetrated into Al2O3Earthenware comes to device Heated, the circle of the operating temperature of sensor, wherein heating coil is regulated and controled by adjusting the operating current size of heater strip Number is that 55 circles, resistance value are 40 Ω.Earthenware is welded on general heater-type hexagonal base and added finally by platinum filament wire Lid protective cover.
(3) finally by sensor in about 200 DEG C of air ambients aging 7 days, so as to obtain graphene/tin ash quantum Point composite material base NO2Gas sensor.
(4) static test system is utilized, sensor is tested at 75 DEG C to 150ppb NO2Response:Sensor is placed in In air atmosphere, sensor heating-up temperature is 75 DEG C;After after sensor resistance stabilization, it is 150ppb's that sensor is placed in into concentration NO2In atmosphere, again wait for sensor resistance and tend towards stability;After the resistance of sensor tends towards stability again, sensor is put In air atmosphere, sensor resistance is waited to return to initial value.
Embodiment 3
(1) graphene/tin dioxide quantal-point composite 0.2g and 2g ethanol that graphene mass fraction is about 2% are taken It is uniformly mixed to form slurry;The slurry is coated uniformly on Al of the surface with a pair of test gold electrodes2O3The surface of earthenware On, make it that gold electrode is completely covered.Wherein the thickness of graphene/tin dioxide quantal-point composite is 15~30um;Al2O3 The internal diameter of earthenware is 0.8mm, and external diameter is 1.2mm, and length is 5mm;The width of single gold electrode is 0.5mm, two gold electrodes Spacing be 0.5mm;The platinum filament wire drawn on gold electrode, its length is 5mm.
(2) earthenware for having coated graphene/tin dioxide quantal-point sensitive material is dried at room temperature for, then by it It is transferred in 80 DEG C of baking ovens and continues to dry 30min.Next nickel-cadmium heating coil is penetrated into Al2O3Earthenware comes to device Heated, the circle of the operating temperature of sensor, wherein heating coil is regulated and controled by adjusting the operating current size of heater strip Number is that 55 circles, resistance value are 40 Ω.Earthenware is welded on general heater-type hexagonal base and added finally by platinum filament wire Lid protective cover.
(3) finally by sensor in about 200 DEG C of air ambients aging 7 days, so as to obtain graphene/tin ash quantum Point composite material base NO2Gas sensor.
(4) static test system is utilized, sensor is tested at 75 DEG C to 250ppb NO2Response:Sensor is placed in In air atmosphere, sensor heating-up temperature is 75 DEG C;After after sensor resistance stabilization, it is 250ppb's that sensor is placed in into concentration NO2In atmosphere, again wait for sensor resistance and tend towards stability;After the resistance of sensor tends towards stability again, sensor is put In air atmosphere, sensor resistance is waited to return to initial value.
Embodiment 4
(1) graphene/tin dioxide quantal-point composite 0.2g and 2g ethanol that graphene mass fraction is about 2% are taken It is uniformly mixed to form slurry;The slurry is coated uniformly on Al of the surface with a pair of test gold electrodes2O3The surface of earthenware On, make it that gold electrode is completely covered.Wherein the thickness of graphene/tin dioxide quantal-point composite is 15~30um;Al2O3 The internal diameter of earthenware is 0.8mm, and external diameter is 1.2mm, and length is 5mm;The width of single gold electrode is 0.5mm, two gold electrodes Spacing be 0.5mm;The platinum filament wire drawn on gold electrode, its length is 5mm.
(2) earthenware for having coated graphene/tin dioxide quantal-point sensitive material is dried at room temperature for, then by it It is transferred in 80 DEG C of baking ovens and continues to dry 30min.Next nickel-cadmium heating coil is penetrated into Al2O3Earthenware comes to device Heated, the circle of the operating temperature of sensor, wherein heating coil is regulated and controled by adjusting the operating current size of heater strip Number is that 55 circles, resistance value are 40 Ω.Earthenware is welded on general heater-type hexagonal base and added finally by platinum filament wire Lid protective cover.
(3) finally by sensor in about 200 DEG C of air ambients aging 7 days, so as to obtain graphene/tin ash quantum Point composite material base NO2Gas sensor.
(4) static test system is utilized, sensor is tested at 75 DEG C to 350ppb NO2Response:Sensor is placed in In air atmosphere, sensor heating-up temperature is 75 DEG C;After after sensor resistance stabilization, it is 350ppb's that sensor is placed in into concentration NO2In atmosphere, again wait for sensor resistance and tend towards stability;After the resistance of sensor tends towards stability again, sensor is put In air atmosphere, the resistance value of sensor is waited to return to initial value.
Embodiment 5
(1) graphene/tin dioxide quantal-point composite 0.3g and 2g ethanol that graphene mass fraction is about 5% are taken It is uniformly mixed to form slurry;The slurry is coated uniformly on Al of the surface with a pair of test gold electrodes2O3The surface of earthenware On, make it that gold electrode is completely covered.Wherein the thickness of graphene/tin dioxide quantal-point composite is 15~30um;Al2O3 The internal diameter of earthenware is 0.8mm, and external diameter is 1.2mm, and length is 5mm;The width of single gold electrode is 0.5mm, two gold electrodes Spacing be 0.5mm;The platinum filament wire drawn on gold electrode, its length is 5mm;
(2) earthenware for having coated graphene/tin dioxide quantal-point sensitive material is dried at room temperature for, then by it It is transferred in 80 DEG C of baking ovens and continues to dry 50min.Next nickel-cadmium heating coil is penetrated into Al2O3Earthenware comes to device Heated, the circle of the operating temperature of sensor, wherein heating coil is regulated and controled by adjusting the operating current size of heater strip Number is that 55 circles, resistance value are 40 Ω.Earthenware is welded on general heater-type hexagonal base and added finally by platinum filament wire Lid protective cover.
(3) finally by sensor in about 300 DEG C of air ambients aging 5 days, so as to obtain graphene/tin ash quantum Point composite material base NO2Gas sensor.
(4) static test system is utilized, sensor is tested at 85 DEG C to 350ppb NO2Response:Sensor is placed in In air atmosphere, sensor heating-up temperature is 85 DEG C;After after sensor resistance stabilization, it is 350ppb's that sensor is placed in into concentration NO2In atmosphere, again wait for sensor resistance and tend towards stability;After the resistance of sensor tends towards stability again, sensor is put In air atmosphere, the resistance value of sensor is waited to return to initial value.

Claims (9)

1. a kind of NO based on graphene/tin dioxide quantal-point composite2Sensor, it is characterised in that described NO2Pass Sensor is heater-type structure, including nickel-cadmium heating coil, Al2O3Earthenware, sensitive layer, Pt wires and two gold electrodes;Institute The nickel-cadmium heating coil stated is located at Al2O3Ceramic tube inside, for heating NO2Sensor;Two gold electrodes are located at Al2O3Pottery The surface of porcelain tube, each gold electrode is connected with Pt wires, by measuring the direct current in different atmosphere between two gold electrodes Hinder resistance and realize measurement NO2The function of concentration;Sensitive layer is wrapped in Al2O3On the outside of earthenware, and two gold electrodes are completely covered;
Described sensitive layer is graphene/tin dioxide quantal-point composite, and thickness is 15~30um;Described Al2O3Ceramics Manage as insulating barrier, its internal diameter is 0.7~0.9mm, external diameter is 1.0~1.5mm, and length is 4~5mm;Described single gold electrode Width be 0.4~0.5mm, the spacing of two gold electrodes is 0.5~0.6mm.
2. a kind of NO based on graphene/tin dioxide quantal-point composite according to claim 12Sensor, it is special Levy and be, the platinum filament wire length drawn on described gold electrode is 4~6mm, and platinum filament wire is by Al2O3Earthenware is welded on logical With on heater-type hexagonal base and being capped protective cover.
3. a kind of NO based on graphene/tin dioxide quantal-point composite according to claim 1 or 22Sensor, Characterized in that, it is 30~40 Ω that the number of turn of described nickel-cadmium heating coil, which is 50~60 circles, resistance value,.
4. the NO based on graphene/tin dioxide quantal-point composite described in the claims 1 or 2 or 32Sensor Preparation method, it is characterised in that following steps:
(1) graphene/tin dioxide quantal-point composite and ethanol are pressed 0.1~0.3:1 mass ratio is well mixed, and is formed Slurry;Slurry is coated uniformly on Al of the surface with a pair of test gold electrodes2O3On the surface of earthenware, it is completely covered Gold electrode;
The coating thickness of described graphene/tin dioxide quantal-point composite is 15~30um;Al2O3The internal diameter of earthenware For 0.7~0.9mm, external diameter is 1.0~1.5mm, and length is 4~5mm;The width of single gold electrode is 0.4~0.5mm, two The spacing of gold electrode is 0.5~0.6mm;
(2) Al of graphene/tin dioxide quantal-point composite will have been coated2O3, will after earthenware placement is dried at room temperature It, which is transferred in 80 DEG C of baking ovens, continues to dry 30~60min;Nickel-cadmium heating coil is penetrated into Al2O3Earthenware is carried out to it Heating, by the operating current size control NO for adjusting heater strip2The operating temperature of sensor;Will finally by platinum filament wire Al2O3Earthenware is welded on general heater-type hexagonal base and is capped protective cover;
(3) by Al2O3Sensor is positioned over aging 5-15 days in 200~400 DEG C of air ambients, obtains graphene/tin ash amount Son point composite material base NO2Gas sensor.
5. the NO according to claim 4 based on graphene/tin dioxide quantal-point composite2The preparation side of sensor Method, it is characterised in that mass fraction of the graphene in graphene/tin dioxide quantal-point composite is 1%-10%.
6. the NO according to claim 4 based on graphene/tin dioxide quantal-point composite2The preparation side of sensor Method, it is characterised in that the platinum filament wire length drawn on described gold electrode is 4~6mm.
7. the NO according to claim 5 based on graphene/tin dioxide quantal-point composite2The preparation side of sensor Method, it is characterised in that the platinum filament wire length drawn on described gold electrode is 4~6mm.
8. the NO according to claim 4 based on graphene/tin dioxide quantal-point composite2The preparation side of sensor Method, it is characterised in that the number of turn of the nickel-cadmium heating coil is that 50~60 circles, resistance value are 30~40 Ω.
9. the NO based on graphene/tin dioxide quantal-point composite according to claim 5 or 62The preparation of sensor Method, it is characterised in that the number of turn of the nickel-cadmium heating coil is that 50~60 circles, resistance value are 30~40 Ω.
CN201710319671.8A 2017-05-09 2017-05-09 A kind of NO based on graphene/tin dioxide quantal-point composite2Sensor and preparation method thereof Pending CN106990142A (en)

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CN108181355A (en) * 2017-12-29 2018-06-19 哈尔滨工业大学 For the preparation method of stannic disulfide/graphene/stannic oxide tri compound gas sensitive of nitrogen dioxide gas sensor
CN108318510A (en) * 2018-01-09 2018-07-24 山东大学 A kind of platinum/tin oxide nano particles cluster gas sensor and preparation method thereof of redox graphene package
CN109142467A (en) * 2018-07-23 2019-01-04 杭州电子科技大学 A kind of high sensitive NO2Gas sensor and preparation method thereof
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