CN106596652A - Preparation method of high-sensitivity NO2 gas sensor - Google Patents
Preparation method of high-sensitivity NO2 gas sensor Download PDFInfo
- Publication number
- CN106596652A CN106596652A CN201611111487.6A CN201611111487A CN106596652A CN 106596652 A CN106596652 A CN 106596652A CN 201611111487 A CN201611111487 A CN 201611111487A CN 106596652 A CN106596652 A CN 106596652A
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- preparation
- gas sensor
- graphene
- high sensitivity
- oxalic acid
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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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- 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
Abstract
The invention discloses a preparation method of a high-sensitivity NO2 gas sensor. The preparation method comprises the following steps: (1) preparing WO3/graphene nanocomposites; taking graphene oxide, sulfate salt and tungstate as raw materials and preparing through a hydrothermal method to obtain the WO3/graphene nanocomposites; (2) preparing a NO2 gas sensor; weighing the WO3/graphene nanocomposites and adding the WO3/graphene nanocomposites into a beaker, carrying out ultrasound treatment for 10 minutes to be dissolved completely, absorbing suspension liquid by using a pipette to a plane electrode, and then preparing into a nano-composite based indirectly heated gas sensor. The gas sensor prepared by the method can show good selectivity and high sensitivity for NO2 at lower working temperature, and further has fast response and recovery characteristics, and potential application in the gas sensor with high performances and low power consumption.
Description
Technical field
The present invention relates to belong to function nano material manufacture field, it is more particularly to a kind of to be based on WO3/ graphene nano is combined
High sensitivity NO of material2The preparation method of gas sensor.
Background technology
NO2Gas is the pungent toxic gas of brownish red, and the burning of Fossil fuel can produce substantial amounts of NO2Gas；Suction
NO2Gas major determinant respiratory tract, while having harm to environment, promotes the formation of acid rain, causes water body, soil and air dirty
Dye；NO is detected at present2The method of gas has spectrophotography, fluorimetry etc..But detect complex operation, testing time length,
Instrument maintenance is costly, and can not carry out field monitoring；Therefore to NO2The quick of gas accurately tests significant；Change
Nano materials are learned to NO2The monitoring of gas is extensively closed because having the advantages that quick, simple to operate, sensitivity is high by people
Note.
Graphene is with sp with carbon atom2The monolayer carbon structure of hydridization, there is high mechanical force (＞ 1060GPa), high heat
The property led (- 3000WM-1K-1), high electron mobility (15000cm2v-1s-1), high-specific surface area (2600m2/g)；Based on high
Electron mobility and big specific surface area, Graphene is a kind of very promising p-type gas sensitive；While WO3As one
N-type material is planted, also there is very wide purposes in terms of air-sensitive test；Gas sensitive is applied to having been reported with Graphene, although
Can work at a lower temperature, but gas-selectively is poor, longer response time and recovery time, and sensitivity compared with
It is low, while WO3It is single as gas sensitive, preferable selectivity and high spirit typically can be shown at higher operating temperatures
Sensitivity.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of being directed to present in existing single gas sensitive sensor not
Foot, reaches to NO by the way that two kinds of system materials are compound2Gas has highly sensitive detection, and the base of excellent selectivity and stability
In WO3High sensitivity NO of/graphene nanocomposite material2The preparation method of gas sensor.
To reach above-mentioned purpose, technical scheme is as follows：
One kind is based on WO3High sensitivity NO of/graphene nanocomposite material2The preparation method of gas sensor, the system
Preparation Method includes：
(1)WO3The preparation of/graphene nanocomposite material
With graphene oxide, sulfate radical salt, tungstates as raw material, WO is prepared by hydro-thermal method3/ graphene nano is multiple
Condensation material；
(2) preparation of gas sensor
Weigh WO3/ graphene nanocomposite material is added in beaker, and ultrasound dissolving in 10 minutes is complete, is inhaled with liquid-transfering gun
Suspension is taken in plane electrode, the heater-type gas sensor of nano combined base is prepared into.
In one embodiment of the invention, the graphene oxide in the claim 1 is prepared by following methods：
Prepared using improved Hummers methods, weigh 1.5g graphite powders, 9g KMnO4, the dense H of 180ml2SO4, 20ml
H3PO4(VH2SO4:VH3PO4=9:1) 500ml round-bottomed flasks are added to, 50 DEG C are heated to, stirring reaction 12h is generated coffee-like molten
Liquid, is cooled to room temperature, pours Deca 3ml 30%H into2O2200ml frozen water in, become brown color suspension；Centrifugation, outwells
Clear liquid, adds dense HCl, and after rocking uniformly, centrifugation is then cleaned multiple times with ethanol and deionized water, treats that supernatant is close to neutrality
Shi Qingxi is completed, and is put into 80 DEG C of baking oven overnight.
In one embodiment of the invention, the tungstates is H2WO4/ oxalic acid vitreosol, the H2WO4/ oxalic acid is saturating
The preparation method of bright colloidal sol is as follows：
By 8.15g Na2WO4Stirring is dissolved in 20ml deionized waters, and enriching HCl, solution is subsequently adding grass into milky
Acid, into transparent, stable H after stirring2WO4/ oxalic acid vitreosol.
In one embodiment of the invention, WO3The concrete preparation method of/graphene nanocomposite material is as follows：
Weigh 5-20mg graphene oxides to be added in beaker, ultrasonic 10min dissolvings are complete, add sulfate radical salt and surpass
Sound, Deca H2WO4/ oxalic acid vitreosol, reacts 8h, prepares WO3/ graphene nanocomposite material.
In one embodiment of the invention, the concrete preparation method of the gas sensor is as follows：
Plane electrode is welded in the substrate of pedestal, 10mg WO are weighed3/ graphene nanocomposite material is added to
In 10ml deionized waters and sonic oscillation 30-60min, finely dispersed WO is obtained3/ graphene nanocomposite material suspension,
Suspension liquid-transfering gun is crossed and is added drop-wise in the plane electrode being welded, make heater-type gas sensor, drying at room temperature 8h,
The sensor electrode of preparation is in heat treatment.
In one embodiment of the invention, the amount of the dense HCl is any one in 4ml, 5ml, 6ml, 7ml or 8ml.
In one embodiment of the invention, the sulfate radical salt is K2SO4、ZnSO4、(NH4)2SO4Or CuSO4In appoint
Meaning is a kind of.
In one embodiment of the invention, the H2WO4The amount of/oxalic acid vitreosol is 12ml, 14ml, 16ml, 18ml
Or any one in 20ml.
In one embodiment of the invention, the temperature during reaction is 120 DEG C, 140 DEG C, 160 DEG C, 180 DEG C or 200
Any one in DEG C.
In one embodiment of the invention, the temperature during heat treatment be 100 DEG C, 120 DEG C, 140 DEG C, 160 DEG C or
Any one in 180 DEG C, the time of the heat treatment is any one in 12h, 24h, 36h, 48h or 60h.
By above-mentioned technical proposal, the invention has the beneficial effects as follows：
The present invention is based on WO3High sensitivity NO of/graphene nanocomposite material2Gas sensing material, it is characterised in that adopt
With two kinds of different type gas sensitives, the gas sensitive that p-type is combined with n-type semiconductor is prepared using hydro-thermal method, for carrying
Rise detection sensitivity, selectivity and the response-recovery time of sensitive material.
Its principle is：
(1) n-type semiconductor WO3It is combined with p-type material Graphene, bi-material is because intermolecular Van der Waals force
Contact, in material contact surface p-n heterojunction can be formed, and because the hetero-junctions energy rank for being formed is relatively low, electronics is easy to from N-shaped partly lead
Body material WO3Upper migration is simultaneously confined to hetero-junctions, and electron motion now will not receive the collision of impurity and be restricted mobility
Can become big.
(2) in n-type semiconductor WO3With the dynamic of carrier occurs at p-type material Graphene composite surface hetero-junctions
State is balanced, while remaining negative ions can be formed in electric field in one, in the presence of electric field, can make carrier toward diffusion phase
Anti- direction is moved and forms depletion layer, and depletion layer broadens can improve the sensitivity of composite.
(3) composite has sizable specific surface area, can adsorb more oxygen, is conducive to molecular state O2-In WO3Table
The quick diffusion in face, NO2Gas will obtain electronics in composite material surface, and this process can improve WO3Surface voids concentration, has
There is quick response and recovery characteristics beneficial to lower temperature lower sensor.In the present invention, the hydro-thermal method synthetic technology for being adopted
It is primarily referred to as in advance H2WO4Presoma is dispersed in oxalic acid solution, then by the temperature of reaction system, addition template agent etc.
Means are by WO3It is nanocrystalline to separate out from solution, while graphene oxide is reduced into Graphene；Made using intermolecular Van der Waals force
WO3Nanocrystalline in-situ deposition is in the surface of Graphene sensitive material；WO3The nanocrystalline tamped density in graphenic surface can lead to
Peroxidating Graphene addition is controlling；By the graphene oxide of Different adding amount, and optimize reaction condition, oxidation can be made
Graphene reduction is thorough, and WO3Uniform nano wire can be formed, the controllable composite nano materials of pattern and valence state are prepared.
The present invention is by the compound of bi-material so that the NO for preparing2Gas sensor can be right at a lower temperature
NO2Gas has very high sensitivity, to 20ppm NO at 100 DEG C265.623 are reached, while when showing very fast response
Between and recovery time, respectively 10s and 126s；By the NO for testing variable concentrations2(5,10,15,20,25,30ppm) gas can
0.958 can be reached with the discovery sensor linearity, to sensor follow-on test 10ppm NO2Adsorption desorption experiment it can be found that pass
Sensor shows good repeatability, and long-time stability experiment is done to transducer sensitivity finds out, transducer sensitivity tool
There is good stability.
Description of the drawings
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
The accompanying drawing to be used needed for having technology description is briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is WO of the present invention3/ graphene nanocomposite material is at a temperature of different operating to 20ppm NO2Sensitivity
Figure；
Fig. 2 is the WO that the present invention adds different amounts of graphene oxide to prepare3The scanning electricity of/graphene nanocomposite material
Mirror photo；
Fig. 3 is WO of the present invention3/ graphene nanocomposite material is to 20ppm NO2The response-recovery curve chart of gas；
Fig. 4 is WO of the present invention3The selection figure of/graphene nanocomposite material to gas with various；
Fig. 5 is WO of the present invention3/ graphene nanocomposite material to variable concentrations (5,10,15,20,25,30ppm) NO2Gas
Body response recovers figure；
Fig. 6 is WO of the present invention3/ graphene nanocomposite material is to 10ppm NO2The reperformance test curve chart of gas；
Fig. 7 is WO of the present invention3/ graphene nanocomposite material is to 20ppm NO2The long term stability tests of gas.
Specific embodiment
In order that technological means, creation characteristic, reached purpose and effect that the present invention is realized are easy to understand, tie below
Conjunction is specifically illustrating, and the present invention is expanded on further.
Embodiment 1
The invention discloses a kind of be based on WO3High sensitivity NO of/graphene nanocomposite material2The system of gas sensor
Preparation Method, preparation method includes：
(1) preparation of graphene oxide
Prepared using improved Hummers methods, weigh 1.5g graphite powders, the dense H of 9g KMnO4,180ml2SO4, 20ml
H3PO4(VH2SO4:VH3PO4=9:1) in being added to 500ml round-bottomed flasks, 50 DEG C of stirring reactions 12h are heated to, are generated coffee-like
Solution, is cooled to room temperature, pours Deca 3ml 30%H into2O2200ml frozen water in, become brown color suspension, be centrifuged, outwell
Supernatant, adds dense HCl, and after rocking uniformly, centrifugation is then cleaned multiple times with ethanol and deionized water, in treating that supernatant is close to
Property when cleaning complete, be put into 80 DEG C of baking oven overnight.
(2) H is prepared2WO4/ oxalic acid vitreosol
By 8.15g Na2WO4Stirring is dissolved in 20ml deionized waters, enriching HCl 6ml, solution milky, adds 6.3g careless
Acid, into transparent, stable colloidal sol after stirring.
(3)WO3The preparation of/graphene nanocomposite material
Weigh 5mg graphene oxides to be added in beaker, ultrasonic 10min dissolvings are complete, add 4g amine sulfates and ultrasound, drop
Plus 16ml H2WO4/ oxalic acid vitreosol, at 180 DEG C 8h is reacted.
(4)NO2The preparation of gas sensor
Plane electrode is welded in the substrate of pedestal, WO prepared in 10mg embodiments one is weighed3/ graphene nano
Composite is added in 10ml deionized waters and sonic oscillation 30-60min, obtains finely dispersed WO3/ graphene nano is multiple
Condensation material suspension, drop coating is crossed to the plane electrode being welded by suspension liquid-transfering gun, makes heater-type gas sensor,
Drying at room temperature 8h, prepare sensor electrode at 120 DEG C heat treatment 24h, to prepare WO3/ graphene nano composite wood
Material is in different operating temperature to 20ppm NO2The sensitivity of gas, its test curve is shown in Fig. 1 L1.
Embodiment 2
The step of embodiment 1 in (3), 10mg graphene oxides, phase in other steps and condition and embodiment 1 are added
Together, actual conditions is made corresponding variation in the range of the content of the invention is limited and is adjusted, and can obtain WO3/ graphene nano is multiple
Condensation material；Graphene nanocomposite material hanging drop is coated onto in the plane electrode being welded, heater-type gas sensing is made
Device, drying at room temperature 8h, prepare sensor electrode at 120 DEG C heat treatment 24h；To the WO for preparing3/ graphene nano is combined
Material is in different operating temperature to 20ppm NO2The sensitivity of gas, its test curve is shown in Fig. 1 L2.
Embodiment 3
The step of embodiment 1 in (3), 15mg graphene oxides, phase in other steps and condition and embodiment 1 are added
Together, actual conditions is made corresponding variation in the range of the content of the invention is limited and is adjusted, and can obtain WO3/ graphene nano is multiple
Condensation material；Graphene nanocomposite material hanging drop is coated onto in the plane electrode being welded, heater-type gas sensing is made
Device, drying at room temperature 8h, prepare sensor electrode at 120 DEG C heat treatment 24h；To the WO for preparing3/ graphene nano is combined
Sensitivity of the material in different operating temperature to 20ppm NO2 gases, its test curve is shown in Fig. 1 L3.
Embodiment 4
The step of embodiment 1 in (3), 20mg graphene oxides, phase in other steps and condition and embodiment 1 are added
Together, actual conditions is made corresponding variation in the range of the content of the invention is limited and is adjusted, and can obtain WO3/ graphene nano is multiple
Condensation material, graphene nanocomposite material hanging drop is coated onto in the plane electrode being welded, and makes heater-type gas sensor,
Drying at room temperature 8h, prepare sensor electrode at 120 DEG C heat treatment 24h, to prepare WO3/ graphene nano composite wood
Material is in different operating temperature to 20ppm NO2The sensitivity of gas, its test curve is shown in Fig. 1 L4.
Embodiment 5
On the basis of embodiment 2, to WO3/ graphene nanocomposite material makees SEM signs, and its microstructure is as schemed
2。
Embodiment 6
WO is obtained during embodiment 23/ graphene nanocomposite material, it is right at 100 DEG C to composite
20ppm NO2The response-recovery curve of gas, its response-recovery curve such as Fig. 3.
Embodiment 7
WO is obtained during embodiment 23/ graphene nanocomposite material, it is right at 100 DEG C to composite
The gas with various test compound material selectivity energy of 20ppm, it selects performance such as Fig. 4.
Embodiment 8
WO is obtained during embodiment 23/ graphene nanocomposite material, to composite variable concentrations NO is carried out2
Tested, checked the linearity of composite, its linearity such as Fig. 5.
Embodiment 9
WO is obtained during embodiment 23/ graphene nanocomposite material, to composite same concentrations NO are carried out2
Tested, checked the repeatability of composite, its response-recovery curve such as Fig. 6.
Embodiment 10
WO is obtained during embodiment 23/ graphene nanocomposite material, to composite long-time stability are carried out
Test, checks the stability of composite, its change of sensitivity such as Fig. 7.
The ultimate principle and principal character and advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel it should be appreciated that the present invention is not restricted to the described embodiments, the simply explanation described in above-described embodiment and description this
The principle of invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, these changes
Change and improvement is both fallen within scope of the claimed invention.The claimed scope of the invention by appending claims and its
Equivalent thereof.
Claims (10)
1. a kind of high sensitivity NO2The preparation method of gas sensor, it is characterised in that the preparation method includes：
(1)WO3The preparation of/graphene nanocomposite material
With graphene oxide, sulfate radical salt, tungstates as raw material, WO is prepared by hydro-thermal method3/ graphene nano composite wood
Material；
(2)NO2The preparation of gas sensor
Weigh WO3/ graphene nanocomposite material is added in beaker, and ultrasound dissolving in 10 minutes is complete, is drawn with liquid-transfering gun and is suspended
Liquid is prepared into the heater-type gas sensor of nano combined base in plane electrode.
2. a kind of base high sensitivity NO according to claim 12The preparation method of gas sensor, it is characterised in that described
Graphene oxide in claim 1 is prepared by following methods：
Prepared using improved Hummers methods, weigh 1.5g graphite powders, 9g KMnO4, the dense H of 180ml2SO4, 20ml H3PO4
(VH2SO4:VH3PO4=9:1) 500ml round-bottomed flasks are added to, 50 DEG C are heated to, stirring reaction 12h generates coffee-like solution, cold
But to room temperature, Deca 3ml 30%H are poured into2O2200ml frozen water in, become brown color suspension；Centrifugation, outwells supernatant,
Dense HCl is added, after rocking uniformly, centrifugation is then cleaned multiple times with ethanol and deionized water, is cleaned when supernatant is close to neutral
Complete, be put into 80 DEG C of baking oven overnight.
3. a kind of high sensitivity NO according to claim 12The preparation method of gas sensor, it is characterised in that the tungsten
Hydrochlorate is H2WO4/ oxalic acid vitreosol, the H2WO4The preparation method of/oxalic acid vitreosol is as follows：
By 8.15g Na2WO4Stirring is dissolved in 20ml deionized waters, and enriching HCl, solution is subsequently adding oxalic acid into milky, stirs
Into transparent, stable H after mixing2WO4/ oxalic acid vitreosol.
4. a kind of high sensitivity NO according to claim 32The preparation method of gas sensor, it is characterised in that WO3/ stone
The concrete preparation method of black alkene nano composite material is as follows：
Weigh 5-20mg graphene oxides to be added in beaker, ultrasonic 10min dissolvings are complete, add sulfate radical salt and ultrasound, drop
Plus H2WO4/ oxalic acid vitreosol, reacts 8h, prepares WO3/ graphene nanocomposite material.
5. a kind of high sensitivity NO according to claim 12The preparation method of gas sensor, it is characterised in that described
NO2The concrete preparation method of gas sensor is as follows：
Plane electrode is welded in the substrate of pedestal, 10mg WO are weighed3/ graphene nanocomposite material be added to 10ml go from
In sub- water and sonic oscillation 30-60min, finely dispersed WO is obtained3/ graphene nanocomposite material suspension, by suspension
Crossed with liquid-transfering gun and be added drop-wise in the plane electrode being welded, make heater-type gas sensor, drying at room temperature 8h, the biography for preparing
Sensor electrode is in heat treatment.
6. a kind of high sensitivity NO according to claim 22The preparation method of gas sensor, it is characterised in that described dense
The amount of HCl is any one in 4ml, 5ml, 6ml, 7ml or 8ml.
7. a kind of high sensitivity NO according to claim 1 or 42The preparation method of gas sensor, it is characterised in that institute
Sulfate radical salt is stated for K2SO4、ZnSO4、(NH4)2SO4Or CuSO4In any one.
8. a kind of high sensitivity NO according to claim 42The preparation method of gas sensor, it is characterised in that described
H2WO4The amount of/oxalic acid vitreosol is any one in 12ml, 14ml, 16ml, 18ml or 20ml.
9. a kind of high sensitivity NO according to claim 42The preparation method of gas sensor, it is characterised in that described anti-
Seasonable temperature is any one in 120 DEG C, 140 DEG C, 160 DEG C, 180 DEG C or 200 DEG C.
10. a kind of high sensitivity NO according to claim 52The preparation method of gas sensor, it is characterised in that described
Temperature during heat treatment is any one in 100 DEG C, 120 DEG C, 140 DEG C, 160 DEG C or 180 DEG C, and the time of the heat treatment is
Any one in 12h, 24h, 36h, 48h or 60h.
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| CN109629228A (en) * | 2018-12-19 | 2019-04-16 | 苏州大学 | A kind of multifunctional fabric and its preparation method and application |
| US10768135B2 (en) | 2017-12-27 | 2020-09-08 | Industrial Technology Research Institute | Oxidizing gas detection method and apparatus thereof |
| WO2021203804A1 (en) * | 2020-04-10 | 2021-10-14 | 中国石油化工股份有限公司 | Self-heating gas sensor, gas-sensitive material, preparation method for same, and applications thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2021203804A1 (en) * | 2020-04-10 | 2021-10-14 | 中国石油化工股份有限公司 | Self-heating gas sensor, gas-sensitive material, preparation method for same, and applications thereof |
| JP7445016B2 (en) | 2020-04-10 | 2024-03-06 | 中国石油化工股▲ふん▼有限公司 | Self-heating gas sensor, gas-sensitive material, manufacturing method and use thereof |
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