CN111307876A - Gas sensor for detecting nitrogen dioxide and preparation method thereof - Google Patents
Gas sensor for detecting nitrogen dioxide and preparation method thereof Download PDFInfo
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- CN111307876A CN111307876A CN201811514190.3A CN201811514190A CN111307876A CN 111307876 A CN111307876 A CN 111307876A CN 201811514190 A CN201811514190 A CN 201811514190A CN 111307876 A CN111307876 A CN 111307876A
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- 239000007789 gas Substances 0.000 title claims abstract description 60
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 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 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000010410 layer Substances 0.000 claims abstract description 43
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 18
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 13
- 239000010703 silicon Substances 0.000 claims abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 11
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 11
- 239000000758 substrate Substances 0.000 claims abstract description 11
- 239000002356 single layer Substances 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 230000001590 oxidative effect Effects 0.000 claims abstract description 4
- 238000001259 photo etching Methods 0.000 claims abstract description 3
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 230000004044 response Effects 0.000 abstract description 11
- 230000035945 sensitivity Effects 0.000 abstract description 7
- 238000001514 detection method Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 3
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 7
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 7
- 230000008859 change Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229920002120 photoresistant polymer Polymers 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000001459 lithography Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000010223 real-time analysis Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention discloses a gas sensor for detecting nitrogen dioxide and a preparation method thereof. The sensor has a multilayer film structure and comprises a silicon-based substrate, an insulating layer, an electrode layer and a gas sensitive layer, wherein the gas sensitive layer comprises graphene and a single-layer MoS compounded on the surface of the graphene2A film. The preparation method comprises the following steps: (1) cleaning the silicon wafer substrate; (2) thermally oxidizing the silicon wafer to generate a silicon oxide insulating layer; (3) forming an electrode pattern layer on the silicon oxide insulating layer by using a photoetching process; (4) forming a graphene layer on the electrode layer; (5) forming a single layer of MoS on a graphene layer2A material. Gas sensor pair NO of the invention2The gas has the advantages of low detection limit, high sensitivity, low response time and the like. The gas sensor has the characteristics of simple structure, compatibility with the existing silicon-based electronic device preparation technology, low-temperature and low-cost preparation and the like.
Description
Technical Field
The invention relates to a gas sensor for detecting nitrogen dioxide and a preparation method thereof, belonging to the technical field of sensors.
Background
Environmental issues are becoming more prominent as our economic construction has achieved significant success. IINitrogen oxide is an air pollutant and can detect NO in real time2The gas has important significance for environmental protection. With the development requirements of the fields of scientific and technological progress, environmental protection and the like, a high-sensitivity novel gas sensor receives extensive attention. Compared with the traditional gas sensor, the novel sensor has the characteristics of high sensitivity, small size, portability, real-time analysis, convenience for batch manufacturing and the like. To improve the performance of gas sensors, researchers have done a lot of meaningful work, mainly focusing on several aspects: lowering the detection limit of the sensor; the sensitivity of the sensor is improved; reducing the response time of the sensor.
In order to improve the performance of the gas sensor, researchers add gas-sensitive materials into the gas sensor, and the performance of the sensor can be obviously enhanced by utilizing the characteristic that the gas-sensitive materials and certain specific gases are physically or chemically adsorbed. In the past decades, researchers have found that some semiconductor materials can cause a change in resistance when contacted with a gas at high temperatures, and have produced a number of highly efficient gas sensors based on the use of sensitive materials based on semiconducting metal oxides, such as SnO2、ZnO、Fe2O3And the like. Graphene has incomparable advantages in gas sensing applications compared with other materials, and is receiving wide attention. The work of graphene-based gas sensors has made preliminary results, and in the current research, due to the diversity of the methods for obtaining graphene materials and the differences in the process of manufacturing graphene sensing samples, each graphene is enabled to do NO2Have different response and recovery characteristics. Therefore, improvement of graphene-based gas sensors is an important direction in which they can be commercially applied.
Disclosure of Invention
The inventors have found, based on an understanding of the mechanism of the sensitive thin film for gas detection, that the choice of the material of the sensitive layer may be crucial, which directly determines the detection sensitivity of the gas sensing device. It is an object of the present invention to provide a gas sensor for detecting nitrogen dioxide, which sensor selects NO2The material with specific reaction and sensitivity is used as a sensitive material, and the NO response of the sensor can be obviously improved2Medicine for treating gasSensitivity and selectivity.
Another object of the present invention is to provide a method for manufacturing the sensor, which is simple and has low manufacturing cost.
In order to achieve the purpose, the invention adopts the following technical scheme:
a gas sensor for detecting nitrogen dioxide is provided with a multilayer film structure and comprises a silicon-based substrate, an insulating layer, an electrode layer and a gas sensitive layer, wherein the gas sensitive layer is provided with graphene and a single-layer MoS compounded on the surface of the graphene2A film.
The invention is through the reaction of NO2MoS with gas-sensitive graphene surface forming monolayer2Materials to enhance sensor pair NO2Sensitivity and selectivity of the gas. Molybdenum disulfide (MoS)2) The molybdenum disulfide is a typical sulfur compound, the single-layer molybdenum disulfide is a graphene-like material, and the special structure and the excellent performance enable the molybdenum disulfide to be widely applied to the fields of tribology, electrochemistry, optics and the like. The surface of the molybdenum disulfide is of a porous structure and has a large specific surface area, so that the molybdenum disulfide has remarkable adsorption capacity and can be used for gas-sensitive materials to remarkably improve the performance of the existing sensor.
A preparation method of the gas sensor for detecting nitrogen dioxide comprises the following steps:
(1) cleaning the silicon wafer substrate;
(2) thermally oxidizing the silicon wafer to generate a silicon oxide insulating layer;
(3) forming an electrode pattern layer on the silicon oxide insulating layer by using a photoetching process;
(4) forming a graphene layer on the electrode layer;
(5) forming a single layer of MoS on a graphene layer2A material.
The invention has the advantages that:
gas sensor pair NO of the invention2The gas has the advantages of low detection limit, high sensitivity, low response time and the like.
The gas sensor has the characteristics of simple structure, compatibility with the existing silicon-based electronic device preparation technology, low-temperature and low-cost preparation and the like.
Drawings
FIG. 1 is a schematic view of a process for manufacturing a gas sensor according to the present invention.
Fig. 2 is a schematic diagram of the operation of the gas sensor of the present invention.
Fig. 3 is a gas sensitive response curve of the gas sensor fabricated in example 1.
Fig. 4 is a response time curve of the gas sensor fabricated in example 1.
Detailed Description
The present invention is further described in detail below with reference to the drawings and examples, but the scope of the present invention is not limited thereto.
As shown in FIG. 1, the gas sensor of the present invention is an electronic device based on a multilayer film structure, and comprises a silicon substrate 101, a silicon oxide medium layer 102 disposed on the silicon substrate 101, an interdigital electrode layer 103 disposed on the silicon oxide medium layer 102, and a graphene layer 104 disposed on the interdigital electrode layer 103, wherein a single-layer MoS is disposed on the graphene layer 1042 Material 105.
Example 1
Specifically, the manufacturing method of the gas sensor comprises the following steps:
step 1: and (5) cleaning the substrate.
A monocrystalline silicon wafer is selected as a substrate material. The cleaning was performed using a standard RCA process: SPM (H)2SO4/H2O2) Removing organic matters, destroying carbon-hydrogen bonds in the organic matters by using strong oxidizing property of sulfuric acid, and soaking the substrate at a ratio of 4:1 at about 130 ℃. APM (NH)4OH/H2O2/H2O) removing the organic compound and the metal elements of IB and IIB groups at the temperature of 70-80 ℃. HPM (HCl/H)2O2/H2O) removing heavy alkali ions and cations at 75-80 ℃.
Step 2: and forming a silicon oxide dielectric layer by thermal oxidation.
And generating a 500-nanometer silicon oxide dielectric layer through a thermal oxidation process.
And step 3: and forming a metal electrode layer.
Forming an interdigital electrode pattern by a standard integrated circuit lithography process: firstly, spin-coating photoresist on the surface of silicon oxide, exposing to form an electrode pattern, depositing Au electrode material by using a physical vapor deposition technology, and removing the photoresist to form an Au interdigital electrode, wherein the thickness of the interdigital electrode is 20 nanometers.
And 4, step 4: and transferring the graphene onto the interdigital electrode layer, wherein the number of the graphene layers is 1-10.
And 5: transfer of monolayer MoS2The material is applied to the graphene layer to form the gas sensing device.
Fig. 2 is a diagram of a testing method of the gas sensor according to embodiment 1 of the present invention, as shown in the figure, we load a voltage on electrodes at two ends of a prototype device of the sensor, test a current change, and obtain monitored gas information.
Fig. 3 is a gas sensitive response curve of the gas sensor fabricated in example 1. When NO is in the gas chamber2When the gas concentration is increased from 0.5ppb to 20ppb, the resistance of the sample changes faster with NO2The gas concentration continues to increase and the change in resistance gradually decreases after the gas concentration exceeds 20 ppb. From the figure, it can be derived that the gas sensor of the present invention is paired with NO2The gas has higher responsivity and sensitivity.
Fig. 4 is a response time curve of the gas sensor fabricated in example 1. In the figure, it can be seen that the device is paired with NO2The response process of the gas is relatively fast, reaching substantially the maximum value of the response in around 250 milliseconds.
Claims (2)
1. The gas sensor for detecting nitrogen dioxide is characterized by having a multilayer film structure and comprising a silicon-based substrate, an insulating layer, an electrode layer and a gas sensitive layer, wherein the gas sensitive layer comprises graphene and a single-layer MoS compounded on the surface of the graphene2A film.
2. A method of manufacturing a gas sensor for detecting nitrogen dioxide as claimed in claim 1, comprising the steps of:
(1) cleaning the silicon wafer substrate;
(2) thermally oxidizing the silicon wafer to generate a silicon oxide insulating layer;
(3) forming an electrode pattern layer on the silicon oxide insulating layer by using a photoetching process;
(4) forming a graphene layer on the electrode layer;
(5) forming a single layer of MoS on a graphene layer2A material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811514190.3A CN111307876B (en) | 2018-12-11 | 2018-12-11 | Gas sensor for detecting nitrogen dioxide and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811514190.3A CN111307876B (en) | 2018-12-11 | 2018-12-11 | Gas sensor for detecting nitrogen dioxide and preparation method thereof |
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| CN111307876A true CN111307876A (en) | 2020-06-19 |
| CN111307876B CN111307876B (en) | 2023-04-14 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112505098A (en) * | 2020-10-29 | 2021-03-16 | 北京机械设备研究所 | MEMS gas sensitive structure and preparation process method thereof |
| CN112946037A (en) * | 2021-04-01 | 2021-06-11 | 岭南师范学院 | Gas sensor and manufacturing method thereof |
| CN114047232A (en) * | 2021-11-25 | 2022-02-15 | 长春工业大学 | Preparation method of resistance type gas sensor based on sheet-shaped composite film |
| CN114166897A (en) * | 2021-11-17 | 2022-03-11 | 中北大学南通智能光机电研究院 | Gas sensor based on graphene microstructure |
| CN114544715A (en) * | 2022-02-24 | 2022-05-27 | 江苏科技大学 | Gas sensor made of graphene-tungsten disulfide composite material and preparation method |
| CN114646419A (en) * | 2022-03-23 | 2022-06-21 | 中山大学 | Gas pressure sensor, preparation method thereof and gas pressure detection method |
| CN116337966A (en) * | 2021-12-15 | 2023-06-27 | 中国科学院大连化学物理研究所 | Gas sensor for detecting gas molecules at high speed and gas detection device and method |
| CN117890441A (en) * | 2024-03-18 | 2024-04-16 | 北京中科海芯科技有限公司 | A gas sensor and a method for manufacturing the same |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112505098A (en) * | 2020-10-29 | 2021-03-16 | 北京机械设备研究所 | MEMS gas sensitive structure and preparation process method thereof |
| CN112946037A (en) * | 2021-04-01 | 2021-06-11 | 岭南师范学院 | Gas sensor and manufacturing method thereof |
| CN114166897A (en) * | 2021-11-17 | 2022-03-11 | 中北大学南通智能光机电研究院 | Gas sensor based on graphene microstructure |
| CN114047232A (en) * | 2021-11-25 | 2022-02-15 | 长春工业大学 | Preparation method of resistance type gas sensor based on sheet-shaped composite film |
| CN116337966A (en) * | 2021-12-15 | 2023-06-27 | 中国科学院大连化学物理研究所 | Gas sensor for detecting gas molecules at high speed and gas detection device and method |
| CN114544715A (en) * | 2022-02-24 | 2022-05-27 | 江苏科技大学 | Gas sensor made of graphene-tungsten disulfide composite material and preparation method |
| CN114646419A (en) * | 2022-03-23 | 2022-06-21 | 中山大学 | Gas pressure sensor, preparation method thereof and gas pressure detection method |
| CN117890441A (en) * | 2024-03-18 | 2024-04-16 | 北京中科海芯科技有限公司 | A gas sensor and a method for manufacturing the same |
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