CN111398368A - Nitrogen dioxide gas sensor based on molybdenum disulfide and preparation method - Google Patents
Nitrogen dioxide gas sensor based on molybdenum disulfide and preparation method Download PDFInfo
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- CN111398368A CN111398368A CN202010367471.1A CN202010367471A CN111398368A CN 111398368 A CN111398368 A CN 111398368A CN 202010367471 A CN202010367471 A CN 202010367471A CN 111398368 A CN111398368 A CN 111398368A
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- 239000007789 gas Substances 0.000 title claims abstract description 62
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 43
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 title claims abstract description 40
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 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 36
- 238000002360 preparation method Methods 0.000 title description 6
- 239000010931 gold Substances 0.000 claims abstract description 24
- 230000004888 barrier function Effects 0.000 claims abstract description 20
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052737 gold Inorganic materials 0.000 claims abstract description 18
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 17
- -1 transition metal sulfide Chemical class 0.000 claims abstract description 16
- 239000000758 substrate Substances 0.000 claims abstract description 15
- 230000008878 coupling Effects 0.000 claims abstract description 5
- 238000010168 coupling process Methods 0.000 claims abstract description 5
- 238000005859 coupling reaction Methods 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 21
- 235000012239 silicon dioxide Nutrition 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 13
- 239000010453 quartz Substances 0.000 claims description 13
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 229920002120 photoresistant polymer Polymers 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000010703 silicon Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 claims description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
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- 238000000151 deposition Methods 0.000 claims description 3
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- 238000007738 vacuum evaporation Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims 2
- 238000001514 detection method Methods 0.000 abstract description 14
- 230000004044 response Effects 0.000 abstract description 5
- 239000010410 layer Substances 0.000 description 38
- 238000003825 pressing Methods 0.000 description 10
- 239000000523 sample Substances 0.000 description 7
- 229910052961 molybdenite Inorganic materials 0.000 description 5
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000011144 upstream manufacturing Methods 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
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- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
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- 229910052681 coesite Inorganic materials 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
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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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- General Health & Medical Sciences (AREA)
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Abstract
The invention relates to the technical field of sensors, and discloses a nitrogen dioxide gas sensor based on molybdenum disulfide, which comprises a box body and a sensor element packaged in the box body, wherein the sensor element comprises a substrate, a barrier layer and an interdigital electrode structure formed by a gold interdigital electrode and a two-dimensional transition metal sulfide layer, wherein the substrate, the barrier layer and the interdigital electrode are sequentially arranged and paved from bottom to top; the box body includes box body and lower box body, go up the box body and connect through dismantling coupling assembling with lower box body. The invention has compact structure, convenient assembly and disassembly, high detection precision, quick response time and small error.
Description
Technical Field
The invention relates to the technical field of sensors, in particular to a nitrogen dioxide gas sensor based on molybdenum disulfide and a preparation method thereof.
Background
With the rapid development of modern industry, a large amount of toxic and harmful gases are emitted, and the problem of environmental air quality has become a great concern for people. Nitrogen dioxide is an important pollutant affecting air quality, mainly from vehicle exhaust emissions and industrial waste gases. High concentrations of nitrogen dioxide cause a number of environmental problems, one of the causes of PM2.5 atmospheric pollution, the major cause of photochemical smog formation, and one of the sources of acid rain. When the concentration exceeds 200 mug/m 3 (equal to about 0.1ppm), nitric oxide can stimulate respiratory organs to cause toxic effects, cause the attack of bronchial diseases and seriously harm human health. Therefore, the development of a nitrogen dioxide gas sensor with high selectivity, high sensitivity and low detection limit to realize high-efficiency detection of nitrogen dioxide gas in the environment has very important significance.
ZnO and SnO are mostly adopted in the traditional semiconductor gas sensor2And the simple metal oxides are sensitive materials, and although the materials have been widely applied in the field of gas sensors, the materials still have certain defects, such as poor selectivity, high working temperature and the like. When flammable and explosive gases are detected, a high working temperature is very easy to become a great potential safety hazard, and the great consequences of target gas combustion and even explosion can be caused, so that the development of the semiconductor gas sensor is limited. In MoS2The represented transition metal chalcogenide (TMDs) two-dimensional material shows great application prospect in the field of room temperature gas sensors due to the unique layered structure and good adsorption property to gas molecules.
In recent years, Yue et al have systematically studied the adsorption of different gas molecules onto a monolayer of MoS2The influence of the electrical properties. Results show H2,O2,NO,NO2Acting as a charge acceptor, resulting in P-type doping; NH (NH)3Acting as charge donors, producing n-type doping these important findings are MoS2Accordingly, L ate et al apply both two-layer and multi-layer MoS2The transistor is used for gas detection, and the detection result is foundWith multiple layers of MoS2Can well realize the control of NO2,NH3And to NH3Has a response effect exactly equal to that of NO2The opposite is true. Therefore, the gas sensor for detecting nitrogen dioxide, which has high detection precision, quick response time and smaller error, is urgently needed to be provided; in addition, the structure of the existing gas sensor is troublesome to install and inconvenient to detach.
Disclosure of Invention
In order to solve the problems, the invention provides a nitrogen dioxide gas sensor based on molybdenum disulfide and a preparation method thereof.
In order to achieve the purpose, the invention provides the following technical scheme:
the utility model provides a nitrogen dioxide gas sensor based on molybdenum disulfide, includes the box body and encapsulates in sensor element in the box body, sensor element includes from supreme base, the barrier layer of arranging in proper order and laying down and gold interdigital electrode structure that gold interdigital electrode and two-dimentional transition metal sulphide layer formed down.
The box body includes box body and lower box body, go up the box body and connect through dismantling coupling assembling with lower box body.
Preferably, the material of the substrate is silicon.
Preferably, the material of the barrier layer is silicon dioxide.
Preferably, the interdigital electrode structure is arranged in two forms, namely, a gold interdigital electrode is positioned above the two-dimensional transition metal sulfide layer, or a gold interdigital electrode is positioned below the two-dimensional transition metal sulfide layer.
Preferably, the material of the two-dimensional transition metal sulfide layer is molybdenum disulfide.
Furthermore, the top of the upper box body is provided with a light source opening, and the periphery of the box body is provided with vent holes.
Furthermore, the lower box body is provided with a hollow cavity for accommodating the sensor element, and elastic cantilevers are arranged around the hollow cavity.
Furthermore, the elastic cantilever comprises a fixed section, a connecting section and a free end, the fixed section is arranged on the inner wall of the cavity, the free end is abutted against the sensor element, and the connecting section is used for connecting the fixed section and the free end.
Further, dismantle coupling assembling and include the spliced pole, follow supreme setting gradually down chuck, spring and clamp plate on the spliced pole, it is protruding that outside salient is provided with the card on the chuck.
The invention provides another technical scheme, and a preparation method of a nitrogen dioxide gas sensor based on molybdenum disulfide comprises the following steps:
step 1: preparing a silicon wafer with the thickness of 400-500 mu m as a substrate, and depositing a barrier layer with the thickness of 200-250 mu m above the silicon wafer;
step 2: weighing quantitative sulfur powder and molybdenum trioxide, then placing the quartz boat, covering a barrier layer above the quartz boat, placing the quartz boat into a single-temperature furnace, setting parameters for heating, wherein the heating temperature is 650-850 ℃, the heating time is 30-40 min, keeping the temperature for 5-10 min, naturally cooling to room temperature, taking out the quartz boat, obtaining a molybdenum disulfide layer on the barrier layer, and introducing nitrogen (70sccm) as protective gas one hour before heating;
and step 3: spin-coating photoresist on the molybdenum disulfide layer in the step 2, photoetching the photoresist to obtain a mask plate, and etching the molybdenum disulfide layer through the mask plate to obtain a molybdenum disulfide layer with a certain shape;
and 4, step 4: removing the residual photoresist in the step (3), heating metal gold (Au) to a certain temperature by utilizing a vacuum evaporation coating process, and evaporating the metal gold (Au) to the surface of the molybdenum disulfide layer to condense and form a film so as to form the required interdigital electrode;
and 5: connecting the copper electrode and the interdigital electrode by using a sticky double-sided copper foil to form an electrode lead wire;
step 6: the substrate is fixed on the switching circuit board through the bracket and then is packaged and protected through the box body. .
Compared with the prior art, the invention has the following beneficial effects:
1) the gas sensor can be used at room temperature under standard atmospheric pressure, the lowest detection limit is less than 100ppb, the response speed is less than 10s, and the quantitative error is less than 15%.
2) The gas sensor provided by the invention is simple to operate and convenient to carry.
3) The periphery of the inner wall of the lower box body of the gas sensor is provided with the elastic cantilever, and the elastic cantilever effectively replaces the prior art that the sensor element is arranged in the shell body in a fixed connecting piece or bonding mode. The elastic cantilever can be directly cut, stamped and bent on a single metal aluminum sheet to be integrally formed, and the manufacturing is convenient; and the sensor element is clamped by the deformation of the elastic cantilever, so that the gas sensor is simple and reliable, and the assembly of the gas sensor is more convenient and faster.
4) The disassembly and connection assembly provided by the invention effectively replaces the connection of the upper shell and the lower shell by screws in the prior art, and solves the problems that the screws need to be assembled or disassembled by means of tools such as a screwdriver and the like during connection, the assembly is troublesome and the disassembly is inconvenient.
Drawings
FIG. 1 is a schematic diagram of an exploded view of a gas sensor according to the present invention;
FIG. 2 is a schematic view of the structure of the gas sensor of the present invention;
FIG. 3 is a side view of a gas sensor of the present invention;
FIG. 4 is a schematic diagram of a sensor element according to the present invention;
FIG. 5 is a schematic view of a disassembled connecting assembly of the present invention;
FIG. 6 is a schematic structural view of a lower case according to the present invention;
FIG. 7 is a schematic structural view of a second connection hole of the present invention;
FIG. 8 is a microscopic view of a two-dimensional transition metal sulfide layer according to the present invention;
FIG. 9 is a graph of the response of a sensor element of the present invention to nitrogen dioxide;
fig. 10 is a graph of IV of a sensor element of the present invention in ohmic contact.
In the figure: the sensor comprises a box body 1, an upper box body 11, a light source port 111, a vent hole 112, a first connecting hole 113, a lower box body 12, an elastic cantilever 121, a containing table 122, a second connecting hole 123, a clamping groove 1231, a notch 124, a detachable connecting component 13, a sensor element 2, a substrate 21, a barrier layer 22, a two-dimensional transition metal sulfide layer 23 and a gold interdigital electrode 24;
the elastic cantilever 121: a fixed section 1211, a connecting section 1212, a free end 1213;
disassembling the connecting assembly 13: the clamping plate 131, the clamping boss 1311, the spring 132, the pressing plate 133, the connecting column 134 and the handle 135.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, other embodiments obtained by persons of ordinary skill in the art without any creative effort belong to the protection scope of the present invention.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. When an element is referred to as being "disposed on" another element, it can be directly on the other element or intervening elements may also be present. The terms "vertical," "horizontal," "left," "right," and the like as used herein are for illustrative purposes only.
Referring to fig. 1 to 10, the invention provides a molybdenum disulfide-based nitrogen dioxide gas sensor, which comprises a box body 1 and a sensor element 2 packaged in the box body 1, wherein the sensor element 2 comprises a substrate 21, a barrier layer 22, and an interdigital electrode structure formed by a gold interdigital electrode 24 and a two-dimensional transition metal sulfide layer 23, which are sequentially arranged and laid from bottom to top; the box body 1 comprises an upper box body 11 and a lower box body 12, wherein the upper box body 11 and the lower box body 12 are connected through a disassembling and connecting assembly 13.
As shown in fig. 1 and 2, the upper case 11 is a rectangular aluminum alloy case, the top of which is provided with a light source opening 111 for light source irradiation, and the periphery of the upper case 11 is provided with a vent hole 112, and the vent hole 112 is a square pore, so that the detection gas can pass through the vent hole conveniently. In addition, a connecting table is formed at four top corners of the upper box body 11, a first connecting hole 113 is formed in the connecting table in a penetrating mode, and a guide groove is formed in the inner wall of the first connecting hole 113 in the axial direction and is used for the disassembling and connecting assembly 13 to penetrate through.
As shown in fig. 6, the lower case 12 is a rectangular aluminum alloy case, which is adapted to the structure of the sensor element 2. And the lower case 12 has a hollow cavity for accommodating the sensor element 2, the sensor element 2 is disposed in the hollow cavity, and the periphery of the hollow cavity is provided with the elastic cantilever 121. The elastic cantilever 121 is arranged in the invention, so that the sensor element 2 is effectively arranged in the shell by a fixed connecting piece or bonding mode in the prior art. The elastic cantilever 121 can be directly cut, stamped and bent on a single metal aluminum sheet to be integrally formed, and the manufacturing is convenient; and rely on the deformation of elastic cantilever 121 to press from both sides tight sensor element 2, simple and reliable makes the equipment of gas sensor more convenient and fast.
Further, in order to enable those skilled in the art to better implement the technical solution of the present invention, the elastic cantilever 121 is described in detail, the elastic cantilever 121 includes a fixed section 1211, a connection section 1212 and a free end 1213, the fixed section 1211 is disposed on the inner wall of the cavity and is integrally formed on the inner wall of the cavity, the free end 1213 abuts against the sensor element 2, and the connection section 1212 is used for connecting the fixed section 1211 and the free end 1213. When the sensor element 2 is mounted in contact with the elastic cantilever 121, the free end 1213 approaches the fixed section 1211, the connecting section 1212 deforms accordingly, and when the sensor element 2 is fitted into the hollow cavity, the connecting section 1212 deforms again, and the free end 1213 moves away from the fixed section 1211, clamping the sensor element 2.
Preferably, the free end 1213 is recessed to form a fixing groove (not shown in the figure) for accommodating the sensor element 2, and by adopting this technical solution, the free end 1213 limits the position of the sensor element 2, so as to prevent the sensor element 2 from sliding out of the free end 1213.
In a further design, a holding platform 122 is arranged below the elastic cantilever 121 and on the bottom surface of the hollow cavity, and the sensor element 2 is erected by the holding platform 122, so that a certain gap is formed between the sensor element 2 and the bottom surface of the hollow cavity, and the influence of the metal shell on the interference of the sensor element 2 and the detection accuracy is avoided. And simultaneously, the sensor element 2 is better contacted with the elastic cantilever 121, so that the clamping of the sensor element 2 in the lower box body 12 is more stable.
In addition, four corners of the lower case 12 are respectively provided with a connecting lug, a second connecting hole 123 corresponding to the first connecting hole 113 is formed on the connecting lug, and a guide groove is also formed on the inner wall of the second connecting hole 123 along the axial direction. And the lower extreme face at connecting hole two 123 upwards has seted up joint groove 1231, and this joint groove 1231 distributes with the guide way on the lower terminal surface of connecting hole two 123 perpendicularly, and its joint groove 1231 is less than the degree of depth of connecting hole two 123 along axial length, can realize the chucking limit to dismantling coupling assembling 13. In addition, a notch 124 for passing out the electrode lead wire is formed on the bottom surface of the lower case 12.
As shown in fig. 5, in order to enable those skilled in the art to better implement the technical solution of the present invention, the disassembling/connecting assembly 13 is described in detail, and the disassembling/connecting assembly 13 is provided to effectively replace the prior art in which a screw is used to connect the upper and lower housings, so as to solve the problems that the prior screw needs to be assembled or disassembled by means of a tool such as a screwdriver, which causes troublesome assembly and inconvenient disassembly. The disassembly connection assembly 13 designed by the technical scheme comprises a connection column 134, a clamping disc 131 sequentially arranged on the connection column 134 from bottom to top, a spring 132 and a pressing plate 133, a clamping protrusion 1311 is outwards protruded on the clamping disc 131, the clamping disc 131 and the connection column 134 are integrally arranged, the spring 132 and the pressing plate 133 are all sleeved on the connection column 134, a handle 135 fixedly connected with one end of the connection column 134, far away from the clamping disc 131, is arranged after the connection column 134 is sleeved with the spring 132 and the pressing plate 133, and is arranged on the connection column 134 in an interference fit mode.
Through adopting above-mentioned technical scheme, when last box body 11 and lower box body 12 connect, align connecting hole 113 and connecting hole two 123, make protruding 1311 of card align the guide way and insert, when the spliced pole 134 takes chuck 131 to insert the lower terminal surface to connecting hole two 123, spring 132 receives the extrusion shrink, rotatory handle 135 makes protruding 1311 of card keep away from the tip of guide way, and get into joint groove 1231, spring 132 is in the state of compressed all the time, make protruding 1311 of card be located joint groove 1231 all the time, thereby make and connect conveniently and be difficult for becoming flexible. The diameter of the pressing plate 133 is larger than that of the first connecting hole 113, one end of the spring 132 abuts against the pressing plate 133, and the pressing plate 133 is tightly attached to the upper end face of the first connecting hole 113.
Preferably, the guide groove and the fastening groove 1231 are dovetail grooves, and the fastening protrusion 1311 corresponds to a dovetail block, so that the contact area between the fastening protrusion 1311 and the fastening groove 1231 is increased, and the fastening is firmer. Further preferably, an elastic member is disposed on the lower end surface of the pressing plate 133 to play a role of buffering; the upper end surface of the pressing plate 133 is provided with a boss, so that a certain gap is reserved between the handle 135 and the pressing plate 133, and the handle 135 can be conveniently held by hand for operation.
Preferably, the material of the substrate 21 is silicon. It is further preferable that the thickness of the substrate 21 is 300 μm to 500 μm.
Preferably, the material of the barrier layer 22 is silicon dioxide. It is further preferred that the thickness of the barrier layer 22 is 200 μm to 300 μm.
Preferably, the material of the two-dimensional transition metal sulfide layer 23 is molybdenum disulfide, and more preferably, the thickness of the two-dimensional transition metal sulfide layer 23 is 200 μm to 300 μm.
The interdigital electrode structure is further configured in two forms, namely, a gold interdigital electrode 24 is positioned above the two-dimensional transition metal sulfide layer 23 to form the surface sensor element 2, or a gold interdigital electrode 24 is positioned below the two-dimensional transition metal sulfide layer 23 to form the intermediate sensor element 2.
The invention provides a preparation method of a nitrogen dioxide gas sensor based on molybdenum disulfide, which comprises the following steps:
step 1: preparing a silicon wafer with the thickness of 300-500 mu m as a substrate 21, and depositing a barrier layer 22 with the thickness of 200-300 mu m above the silicon wafer;
step 2: weighing 0.08-0.1 g of sulfur powder and 0.02-0.04 g of molybdenum trioxide, then placing the quartz boat, covering a barrier layer 22 above the quartz boat, placing the quartz boat in a single-temperature furnace, setting parameters for heating at 650-850 ℃ (650 ℃, 750 ℃ and 850 ℃) for 30-40 min, preserving heat for 5-10 min, naturally cooling to room temperature, taking out the quartz boat, obtaining a molybdenum disulfide layer on the barrier layer 22, and introducing nitrogen (70sccm) as protective gas one hour before heating; or (placing quartz boat containing 0.08g of sulfur powder at the upstream of the single-temperature furnace, placing ceramic boat containing 0.02g of molybdenum trioxide at the downstream of the single-temperature furnace, placing SiO2 barrier layer 22 of step 1 beside the ceramic boat containing molybdenum trioxide, introducing Ar (70sccm) as protective gas one hour before the reaction, heating the upstream and downstream of the single-temperature furnace simultaneously, heating the upstream to 160 ℃ at a speed of 2.7 ℃/min, and heating the downstream to 650 ℃ at a speed of 10.7 ℃/min to obtain a molybdenum disulfide layer with a multi-layer horizontal arrangement structure of about 10 nm)
And step 3: spin-coating photoresist on the molybdenum disulfide layer in the step 2, photoetching the photoresist to obtain a mask plate, and etching the molybdenum disulfide layer through the mask plate to obtain a molybdenum disulfide layer with a certain shape;
and 4, step 4: removing the residual photoresist in the step (3), heating metal gold (Au) to a certain temperature by utilizing a vacuum evaporation coating process, and evaporating the metal gold (Au) to the surface of the molybdenum disulfide layer to condense and form a film so as to form the required interdigital electrode;
and 5: connecting the copper electrode and the interdigital electrode by using a sticky double-sided copper foil to form an electrode lead wire;
step 6: the substrate 21 is fixed on the adapter circuit board through a bracket and then is packaged and protected through the box body 1.
The gas sensor provided by the invention is adopted for detection limit detection:
setting probes at two ends of an electrode lead wire of the nitrogen dioxide gas sensor, placing the electrode lead wire into a sealed container, controlling the concentration of gas in the sealed container through a flowmeter, introducing nitrogen dioxide with the concentration of 0.1ppm into the sealed container, keeping the time of the gas in the sealed container for 10-15 minutes, applying voltage at two ends of the probes, and detecting the current passing through the gas sensor; if the detection can be made, nitrogen dioxide with the concentration of 0ppm, 0.01ppm, 0.02ppm, 0.03ppm, 0.04ppm, 0.05ppm, 0.06ppm, 0.07ppm, 0.08ppm and 0.09ppm is respectively introduced into the closed container, voltage is applied to two ends of the probe, and the current passing through the gas sensor of the invention is detected;
if the nitrogen dioxide can not be detected, introducing nitrogen dioxide with the concentration of 1.0ppm into the closed container, keeping the gas in the closed container for 10-15 minutes, applying voltage to two ends of the probe, and detecting the current passing through the gas sensor; if the concentration of nitrogen dioxide can be detected, nitrogen dioxide with the concentration of 0.20ppm, 0.30ppm, 0.40ppm, 0.50ppm, 0.60ppm, 0.70ppm, 0.80ppm and 0.90ppm is respectively introduced into the closed container, voltage is applied to two ends of the probe, and the current passing through the gas sensor of the invention is detected;
if the nitrogen dioxide can not be detected, introducing nitrogen dioxide with the concentration of 10.0ppm into the closed container, keeping the gas in the closed container for 10-15 minutes, applying voltage to two ends of the probe, and detecting the current passing through the gas sensor; if the current can be detected, respectively introducing nitrogen dioxide with the concentration of 2.0ppm, 3.0ppm, 4.0ppm, 5.0ppm, 6.0ppm, 7.0ppm, 8.0ppm and 9.0ppm into a closed container, applying voltage to two ends of a probe, and detecting the current passing through the gas sensor;
by analogy, the detection limit of the nitrogen dioxide is obtained and is less than 1.0 ppm. And the corresponding speed is high, and the detection result appears within 10s generally. In addition, after comparison, the gas concentration error detected by the gas sensor is small, and the specific quantitative error is less than 15%.
In the description of the present invention, it should be noted that unless otherwise explicitly stated or limited, the terms "mounted," "provided," and "connected" are to be construed broadly, e.g., as being fixedly connected, detachably connected, or integrally connected; can be mechanically connected, can also be electrically connected or can be communicated with each other; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention. It is intended that the invention not be limited to the particular embodiment disclosed, but that the invention will include all embodiments falling within the scope of the appended claims and all equivalents thereof.
Claims (10)
1. The utility model provides a nitrogen dioxide gas sensor based on molybdenum disulfide, includes box body (1) and encapsulates in sensor element (2) in box body (1), its characterized in that: the sensor element (2) comprises a substrate (21), a barrier layer (22) and an interdigital electrode structure formed by a gold interdigital electrode (24) and a two-dimensional transition metal sulfide layer (23), which are sequentially arranged and laid from bottom to top;
the box body (1) comprises an upper box body (11) and a lower box body (12), wherein the upper box body (11) is connected with the lower box body (12) through a disassembling and connecting assembly (13).
2. The molybdenum disulfide based nitrogen dioxide gas sensor of claim 1, wherein: the material of the substrate (21) is silicon.
3. The molybdenum disulfide based nitrogen dioxide gas sensor according to claim 1 or 2, wherein: the material of the barrier layer (22) is silicon dioxide.
4. The molybdenum disulfide based nitrogen dioxide gas sensor of claim 3, wherein: the interdigital electrode structure is arranged in two forms, namely a gold interdigital electrode (24) is positioned above the two-dimensional transition metal sulfide layer (23), or the gold interdigital electrode (24) is positioned below the two-dimensional transition metal sulfide layer (23).
5. The molybdenum disulfide based nitrogen dioxide gas sensor of claim 4, wherein: the material of the two-dimensional transition metal sulfide layer (23) is molybdenum disulfide.
6. The molybdenum disulfide based nitrogen dioxide gas sensor of claim 1, wherein: the top of the upper box body (11) is provided with a light source opening (111), and the periphery of the box body (1) is provided with vent holes (112).
7. The molybdenum disulfide based nitrogen dioxide gas sensor of claim 1, wherein: the lower box body (12) is provided with a hollow cavity for accommodating the sensor element (2), and elastic cantilevers (121) are arranged around the hollow cavity.
8. The molybdenum disulfide based nitrogen dioxide gas sensor of claim 7, wherein: the elastic cantilever (121) comprises a fixed section (1211), a connecting section (1212) and a free end (1213), the fixed section (1211) is arranged on the inner wall of the cavity, the free end (1213) is abutted to the sensor element (2), and the connecting section (1212) is used for connecting the fixed section (1211) and the free end (1213).
9. The molybdenum disulfide based nitrogen dioxide gas sensor according to any one of claims 6 to 8, wherein: dismantle coupling assembling (13) and include spliced pole (134), set gradually from supreme down chuck (131), spring (132) and clamp plate (133) on spliced pole (134), chuck (131) are gone up to the outside protruding card of being provided with protruding (1311).
10. The method for preparing a molybdenum disulfide-based nitrogen dioxide gas sensor as claimed in claim 1, wherein: the method comprises the following steps:
step 1: preparing a silicon wafer with the thickness of 400-500 mu m as a substrate (21), and depositing a barrier layer (22) with the thickness of 200-250 mu m above the silicon wafer;
step 2: weighing quantitative sulfur powder and molybdenum trioxide, then placing the quartz boat, covering a barrier layer (22) above the quartz boat, placing the quartz boat into a single-temperature furnace, setting parameters for heating, wherein the heating temperature is 650-850 ℃, the heating time is 30-40 min, keeping the temperature for 5-10 min, naturally cooling to room temperature, taking out the quartz boat, obtaining a molybdenum disulfide layer on the barrier layer (22), and introducing nitrogen (70sccm) as protective gas one hour before heating;
and step 3: spin-coating photoresist on the molybdenum disulfide layer in the step 2, photoetching the photoresist to obtain a mask plate, and etching the molybdenum disulfide layer through the mask plate to obtain a molybdenum disulfide layer with a certain shape;
and 4, step 4: removing the residual photoresist in the step (3), heating metal gold (Au) to a certain temperature by utilizing a vacuum evaporation coating process, and evaporating the metal gold (Au) to the surface of the molybdenum disulfide layer to condense and form a film so as to form the required interdigital electrode;
and 5: connecting the copper electrode and the interdigital electrode by using a sticky double-sided copper foil to form an electrode lead wire;
step 6: the substrate (21) is fixed on the switching circuit board through a bracket and then is packaged and protected through the box body (1).
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