CN114047232A - Preparation method of resistance type gas sensor based on sheet-shaped composite film - Google Patents
Preparation method of resistance type gas sensor based on sheet-shaped composite film Download PDFInfo
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- CN114047232A CN114047232A CN202111410748.5A CN202111410748A CN114047232A CN 114047232 A CN114047232 A CN 114047232A CN 202111410748 A CN202111410748 A CN 202111410748A CN 114047232 A CN114047232 A CN 114047232A
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- composite film
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- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000002131 composite material Substances 0.000 title claims abstract description 11
- YRZZLAGRKZIJJI-UHFFFAOYSA-N oxyvanadium phthalocyanine Chemical compound [V+2]=O.C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 YRZZLAGRKZIJJI-UHFFFAOYSA-N 0.000 claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000012986 modification Methods 0.000 claims abstract description 11
- 230000004048 modification Effects 0.000 claims abstract description 11
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 9
- 239000011521 glass Substances 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 4
- 230000035945 sensitivity Effects 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims abstract 6
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims abstract 4
- 238000005516 engineering process Methods 0.000 claims abstract 2
- 238000007738 vacuum evaporation Methods 0.000 claims abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 4
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 239000010408 film Substances 0.000 claims 3
- 239000010409 thin film Substances 0.000 claims 1
- 241000405147 Hermes Species 0.000 abstract 1
- 230000004043 responsiveness Effects 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 238000001771 vacuum deposition Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 22
- 239000011259 mixed solution Substances 0.000 description 9
- 239000000243 solution Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 2
- 239000012286 potassium permanganate Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000003915 air pollution Methods 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Classifications
-
- 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
Abstract
The invention relates to a preparation method of a resistance type gas sensor based on a sheet-shaped composite film. The sensor is in a resistor structure and comprises a glass substrate (1), an aluminum Al interdigital electrode (2), a Reduced Graphene Oxide (RGO) modification layer (3) and a vanadyl phthalocyanine (VOPc) gas sensitive layer (4). Aluminum Al interdigital electrodes (2) are firstly evaporated on a glass substrate (1) by a vacuum evaporation technology. Graphene (Gr) is prepared into Graphene Oxide (GO) by an improved Hermes (Hummers) method, an RGO solution is prepared by a hydrazine reduction method, the RGO solution is dripped on an Al interdigital electrode (2), and an RGO modification layer (3) with a sheet thin-layer structure is obtained after drying, so that high specific surface area and adsorption sites are obtained. The VOPc gas sensitive layer (4) is prepared by a vacuum evaporation method to form a sheet-shaped composite film, so that the resistance type gas sensor is obtained, and the responsiveness of the sensor is improved. The gas sensor has the advantages of high sensitivity, working at room temperature and simple preparation process.
Description
Technical Field
The invention discloses a preparation method of a sheet-shaped composite film resistor-based gas sensor, and relates to the field of gas sensors.
Background
With the development of modern society, air pollution caused by harmful gases such as nitrogen dioxide, formaldehyde, sulfur dioxide and the like in factory exhaust gas and automobile exhaust gas is increasing, and even if the harmful gases are in extremely low concentration, irreversible damage can be caused to a human body, so that monitoring of toxic and harmful gases is particularly important.
Although the resistance type gas sensor has been widely used in practice in recent years, it has the advantages of high sensitivity, simple manufacturing, etc., but it still has the disadvantages of short life, poor selectivity, high working temperature, etc., and the improvement of the comprehensive performance of the sensor has become the focus of the current research.
Graphene (Gr) is a promising candidate material for room temperature and high performance gas sensing due to its unique structure and electronic properties. However, the poor selectivity of raw Gr prevents its practical application in nitrogen dioxide detection. Reduced Graphene Oxide (RGO) has good application prospects in gas sensing applications due to its high yield, diversity of surface functional groups, and ease of chemical modification to adjust sensing performance. The RGO thin sheets can be self-assembled into a three-dimensional porous structure and combined with a vanadyl phthalocyanine (VOPc) gas sensitive layer, so that the gas response speed can be better improved, and the detection threshold is lower.
Disclosure of Invention
In order to solve the problems of poor selectivity and high working temperature of the conventional gas sensor, the invention provides a preparation method of a sheet-shaped composite film resistance-type gas sensor.
The invention relates to a resistance type structure gas sensor, which sequentially comprises a glass substrate (1), an aluminum (Al) interdigital electrode (2), a Reduced Graphene Oxide (RGO) modification layer (3) and a vanadyl phthalocyanine (VOPc) gas sensitive layer (4) from bottom to top.
The invention relates to a preparation method of a resistance type gas sensor based on a sheet-shaped composite film, which comprises the following steps:
firstly, 8 is multiplied by 10-4And (2) evaporating Al interdigital electrodes (2) on the glass substrate (1) by using a mask plate under the vacuum condition of Pa to be 200-300 nm.
Then 0.45-0.55 g of graphene is weighed, 40-50 ml of concentrated sulfuric acid (98%) and 10-20 ml of concentrated nitric acid (65%) are weighed, and the weighed materials are dropwise added into a three-necked bottle to form a mixed solution. Weighing 2.5-3.5 g of potassium permanganate, adding into the mixed solution, controlling the temperature below 20 ℃, and keeping for 1.5-2.5 h. Then the temperature of the mixed solution is raised to 30-40 ℃ and kept for 1-1.5 h, and the temperature is raised to 80-90 ℃ and kept for 0.3-0.8 h. 40-50 ml of deionized water is dripped, and the constant temperature of 80-90 ℃ is kept for 0.3-0.8 h. After cooling, 4-6 ml of hydrogen peroxide (30%) is dripped, centrifugal washing is carried out until the p H value is between 5 and 6, and vacuum drying is carried out for 9-11 h at the temperature of 55-65 ℃ to obtain GO.
GO is prepared into 0.5 mg/ml with deionized water-1The solution is subjected to ultrasonic treatment, 80% hydrazine hydrate is dropwise added under the heating condition, the reaction is carried out for 1.5 to 2.5 hours under the water bath of 95 to 100 ℃, then the solution is washed by ethanol and deionized water, vacuum drying is carried out for 11 to 13 hours at the temperature of 50 to 60 ℃, the prepared RGO is dropwise added on the Al interdigital electrode (2) by taking DMF as a solvent through ultrasonic dispersion, and the RGO modification layer (3) is obtained by drying.
Finally, the VOPc gas sensitive layer (4) is evaporated on the basis, and the evaporation speed is 3-4 nm.min-1The thickness is 45-55 nm.
Drawings
FIG. 1: based on the sheet-like compound film resistance type gas sensor structure sketch map.
Detailed Description
1. Preparation of Al interdigital electrode
At 8X 10-4And (3) evaporating an Al interdigital electrode (2) on the glass substrate (1) by using a mask plate under the vacuum condition of Pa to be 250 nm.
2. Preparation of GO
0.5 g Gr is weighed again, 45 ml of concentrated sulfuric acid (98%) and 15 ml of concentrated nitric acid (65%) are weighed, the mixture is added dropwise into a three-necked flask to form a mixed solution, and the mixed solution is slowly stirred to keep the temperature below 10 ℃. 3.0 g of potassium permanganate is weighed and slowly added into the mixed solution of the three-necked bottle, the temperature is controlled below 20 ℃, and the mixed solution is kept in an ice-water bath for 2 hours. Then the temperature of the mixed solution is raised to 35 ℃ and kept for 1 h, and then the temperature is raised to 85 ℃ and kept for 0.5 h. 45 ml of deionized water was added dropwise to the mixed solution, and the temperature was kept constant at 85 ℃ for 0.5 hour. After cooling to room temperature, 5 ml of hydrogen peroxide (30%) is dropwise added, then centrifugal washing is carried out until the p H value is between 5 and 6, and vacuum drying is carried out for 10 h at 60 ℃ to obtain GO.
3. Preparation of RGO modification layer
GO is dispersed in deionized water to be prepared into 0.5 mg-m L-1And carrying out ultrasonic treatment on the solution; fixing the reaction system in an electric oil bath, heating and slowly dropwise adding 80% hydrazine hydrate, and carrying out water bath reaction for 2.5 h at 98 ℃. After the reaction is finished, washing the reaction product by using ethanol and deionized water, and drying the reaction product in vacuum at 60 ℃ for 12 hours. And ultrasonically dispersing the prepared RGO by using DMF as a solvent, dripping the prepared RGO on the Al interdigital electrode (2), and drying to obtain the RGO modified layer (3).
4. Preparation of VOPc gas sensitive layer
Finally, the VOPc gas sensitive layer (4) is evaporated on the basis, and the evaporation speed is 3 nm.min-1And the thickness is 50 nm.
Claims (2)
1. A preparation method based on a sheet-shaped composite film resistor type gas sensor is characterized by comprising the following steps: the resistance device structure comprises a glass substrate (1), an aluminum (Al) interdigital electrode (2), a Reduced Graphene Oxide (RGO) modification layer (3) and a vanadyl phthalocyanine (VOPc) gas sensitive layer (4), wherein the RGO modification layer (3) is prepared by a hydrazine reduction method, and the Al interdigital electrode (2) and the VOPc gas sensitive layer (4) are obtained by a vacuum evaporation technology.
2. The method for preparing a sheet-like composite thin film resistor-based gas sensor according to claim 1, wherein the method comprises the following steps: the composite film consists of an RGO modification layer (3) and a VOPc gas sensitive layer (4), wherein the sheet-shaped RGO modification layer (3) is formed by preparing GO from graphene (Gr) by an improved Hermeis (Hummers) method, and 0.5 mg/ml is prepared from GO and deionized water-1And the solution of (a) is subjected to ultrasonic treatment,then 80% hydrazine hydrate is dripped under the heating condition, the reaction is carried out for 1.5 to 2.5 hours under the water bath of 95 to 100 ℃, then the obtained product is washed by ethanol and deionized water, vacuum drying is carried out for 11 to 13 hours at the temperature of 50 to 60 ℃, the prepared RGO is ultrasonically dispersed by taking DMF as a solvent, the obtained product is dripped on an Al interdigital electrode (2), drying is carried out to obtain an RGO modification layer (3) with a sheet structure, a VOPc gas sensitive layer (4) is evaporated on the RGO modification layer (3), and the evaporation speed is 3 to 4 nm.min-1The thickness is 45-55 nm, the obtained sheet-shaped composite film has high specific surface area and active sites, and the sensitivity of gas detection is improved.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104650517A (en) * | 2014-12-09 | 2015-05-27 | 王瑜玉 | Preparation method of graphene oxide composite material |
| CN105699441A (en) * | 2016-03-24 | 2016-06-22 | 电子科技大学 | Resistance-type gas sensor and manufacturing method thereof |
| CN106680336A (en) * | 2016-11-30 | 2017-05-17 | 常州大学 | Preparation of reduced graphene oxide/zinc phthalocyanine film, and application of film in NO2 gas monitoring |
| CN108231942A (en) * | 2016-12-13 | 2018-06-29 | 中国科学院理化技术研究所 | A kind of oxidation graphene film photodetector and its preparation method and application |
| CN109142446A (en) * | 2018-08-20 | 2019-01-04 | 长春工业大学 | A kind of poroid three-dimensional organic gas sensor preparation method of thin polymer film |
| CN111307876A (en) * | 2018-12-11 | 2020-06-19 | 有研工程技术研究院有限公司 | Gas sensor for detecting nitrogen dioxide and preparation method thereof |
-
2021
- 2021-11-25 CN CN202111410748.5A patent/CN114047232A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104650517A (en) * | 2014-12-09 | 2015-05-27 | 王瑜玉 | Preparation method of graphene oxide composite material |
| CN105699441A (en) * | 2016-03-24 | 2016-06-22 | 电子科技大学 | Resistance-type gas sensor and manufacturing method thereof |
| CN106680336A (en) * | 2016-11-30 | 2017-05-17 | 常州大学 | Preparation of reduced graphene oxide/zinc phthalocyanine film, and application of film in NO2 gas monitoring |
| CN108231942A (en) * | 2016-12-13 | 2018-06-29 | 中国科学院理化技术研究所 | A kind of oxidation graphene film photodetector and its preparation method and application |
| CN109142446A (en) * | 2018-08-20 | 2019-01-04 | 长春工业大学 | A kind of poroid three-dimensional organic gas sensor preparation method of thin polymer film |
| CN111307876A (en) * | 2018-12-11 | 2020-06-19 | 有研工程技术研究院有限公司 | Gas sensor for detecting nitrogen dioxide and preparation method thereof |
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Application publication date: 20220215 |