CN111398366B - Method for improving molybdenum disulfide gas sensor by adopting vanadium and sensing equipment - Google Patents
Method for improving molybdenum disulfide gas sensor by adopting vanadium and sensing equipment Download PDFInfo
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- CN111398366B CN111398366B CN202010367462.2A CN202010367462A CN111398366B CN 111398366 B CN111398366 B CN 111398366B CN 202010367462 A CN202010367462 A CN 202010367462A CN 111398366 B CN111398366 B CN 111398366B
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 145
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 145
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 48
- 239000000758 substrate Substances 0.000 claims abstract description 19
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000005234 chemical deposition Methods 0.000 claims abstract description 5
- 239000010410 layer Substances 0.000 claims description 161
- 239000007789 gas Substances 0.000 claims description 48
- 239000010931 gold Substances 0.000 claims description 27
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 24
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 22
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 17
- 229910052737 gold Inorganic materials 0.000 claims description 17
- 239000010453 quartz Substances 0.000 claims description 16
- 239000002356 single layer Substances 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 13
- 229920002120 photoresistant polymer Polymers 0.000 claims description 12
- 239000010936 titanium Substances 0.000 claims description 12
- 229910021550 Vanadium Chloride Inorganic materials 0.000 claims description 11
- RPESBQCJGHJMTK-UHFFFAOYSA-I pentachlorovanadium Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[V+5] RPESBQCJGHJMTK-UHFFFAOYSA-I 0.000 claims description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 229910052719 titanium Inorganic materials 0.000 claims description 10
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 8
- 239000002390 adhesive tape Substances 0.000 claims description 8
- 229910052697 platinum Inorganic materials 0.000 claims description 8
- 229910052709 silver Inorganic materials 0.000 claims description 8
- 239000004332 silver Substances 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 claims description 6
- 238000005530 etching Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000001259 photo etching Methods 0.000 claims description 4
- 238000004528 spin coating Methods 0.000 claims description 4
- 238000007738 vacuum evaporation Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000011084 recovery Methods 0.000 abstract description 16
- 230000035484 reaction time Effects 0.000 abstract description 8
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 7
- 239000011733 molybdenum Substances 0.000 abstract description 7
- 229910052717 sulfur Inorganic materials 0.000 abstract description 7
- 239000011593 sulfur Substances 0.000 abstract description 7
- 230000002411 adverse Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 16
- 238000003825 pressing Methods 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- 230000004044 response Effects 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 230000035945 sensitivity Effects 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 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 3
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- 239000011540 sensing material Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- -1 transition metal chalcogenide Chemical class 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000004323 axial length Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
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 the technical field of sensors, in particular to a method for improving a molybdenum disulfide gas sensor by adopting vanadium and sensing equipment. The invention provides a method for improving a molybdenum disulfide gas sensor by adopting vanadium, which comprises the following steps: preparing a substrate; preparing a dielectric layer on a substrate by using a chemical deposition method; preparing a vanadium-doped molybdenum disulfide layer on the dielectric layer; preparing an interdigital electrode on the vanadium-doped molybdenum disulfide layer; the interdigital electrode is connected with the external pin. The invention also provides sensing equipment which comprises a box body and a sensor prepared by the method for improving the molybdenum disulfide gas sensor by adopting vanadium. By adopting the scheme, the vanadium (V) is used for doping the molybdenum disulfide layer, so that adverse effects caused by molybdenum vacancies and sulfur vacancies are overcome, the reaction time of the sensor can be shortened, and the recovery time can be reduced.
Description
Technical Field
The invention relates to the technical field of sensors, in particular to a method for improving a molybdenum disulfide gas sensor by adopting vanadium and sensing equipment.
Background
The traditional semiconductor gas sensor mostly adopts ZnO and SnO 2 The simple metal oxides are sensitive materials which are already widely available in the field of gas sensorsBut still have certain disadvantages such as poor selectivity, high operating temperature, etc. When detecting flammable and explosive gases, the higher working temperature is very likely to become a serious potential safety hazard, and can cause serious consequences of target gas combustion and even explosion, thereby limiting the development of the semiconductor gas sensor. With molybdenum disulfide (MoS) 2 ) Representative transition metal chalcogenide (TMDs) two-dimensional materials are directed to gas molecules such as NO due to their unique layered structure 2 、NO、NH 3 The gas shows good adsorption characteristics, so that the gas has great application prospect in the field of room temperature gas sensors.
MoS 2 As a highly efficient gas sensing material, there is a great interest in detecting gas at room temperature without a heating device, and at the same time, moS 2 The material can also be used as a light sensing material and can be applied to the light sensing material. Some theoretical calculations confirm that the gas is adsorbed to MoS in the form of physical adsorption 2 Surface, which means gas versus MoS 2 Is a very short process. However, hydrothermally and other wet synthesized MoS 2 There is no theoretical predicted fast response/recovery behavior when the gas is detected at room temperature. This is because of the MoS synthesized by the hydrothermal method 2 The presence of more or less defects (e.g. molybdenum vacancies, sulfur vacancies) on the surface is not an ideal uniform surface in theoretical calculations. These defects lead to MoS 2 Chemical adsorption with gas molecules is strong, so that the gas molecules are difficult to separate from MoS 2 And (5) surface desorption. MoS (MoS) 2 The difficulty in desorption at room temperature results in a slower response/recovery time at room temperature, even without recovery, which greatly hinders the practical application of molybdenum disulfide gas sensors.
Therefore, there is a need in the art for a method and sensing apparatus for improving molybdenum disulfide gas sensors using vanadium.
In view of this, the present invention has been proposed.
Disclosure of Invention
The invention aims to provide a method for improving a molybdenum disulfide gas sensor by adopting vanadium and sensing equipment, so as to solve at least one technical problem.
Specifically, the invention provides a method for improving a molybdenum disulfide gas sensor by adopting vanadium, which comprises the following steps:
preparing a substrate;
preparing a dielectric layer on a substrate by using a chemical deposition method;
preparing a vanadium-doped molybdenum disulfide layer on the dielectric layer;
preparing an interdigital electrode on the vanadium-doped molybdenum disulfide layer;
the interdigital electrode is connected with the external pin.
The substrate can be silicon (Si), ceramic or the like, the dielectric layer can be silicon dioxide, aluminum oxide or the like, the interdigital electrode can be gold (Au), platinum (Pt), silver (Ag) or the like, and the external pin can be copper (Cu), aluminum (Al) or the like.
By adopting the scheme, the vanadium (V) is used for doping the molybdenum disulfide layer, so that adverse effects caused by molybdenum vacancies and sulfur vacancies are overcome, the reaction time of the sensor can be shortened, and the recovery time can be reduced.
Preferably, the preparation of the vanadium-doped molybdenum disulfide layer on the dielectric layer comprises the following steps:
weighing quantitative sulfur powder, molybdenum trioxide and vanadium chloride, and then placing the materials into a quartz boat;
covering a dielectric layer above the quartz boat;
putting the quartz boat into a single-temperature furnace, heating at 650-850 ℃ for 30-40 min under the protection of hydrogen gas, and preserving the heat for 5-10 min;
and naturally cooling to room temperature, taking out the quartz boat, and obtaining a vanadium-doped molybdenum disulfide layer on the dielectric layer.
By adopting the scheme, the molybdenum trioxide can be fully reduced under the action of hydrogen, vanadium is doped with molybdenum vacancies and sulfur vacancies, and the sensitivity of the sensor is improved.
Further, preparing the vanadium-doped molybdenum disulfide layer on the dielectric layer comprises preparing a single-layer molybdenum disulfide layer by a mechanical stripping method.
Preferably, the method for preparing the vanadium-doped molybdenum disulfide layer on the dielectric layer comprises the following steps:
sticking an adhesive tape on the vanadium-doped molybdenum disulfide layer, and tearing the adhesive tape, so that the molybdenum disulfide sheet layer is separated to obtain a thinner vanadium-doped molybdenum disulfide layer;
repeating the steps;
and detecting the number of layers of molybdenum disulfide by using an instrument, and stopping repeating when a single vanadium-doped molybdenum disulfide layer is obtained.
By adopting the technical scheme, a single vanadium-doped molybdenum disulfide layer is obtained, and the applicability of the sensor is improved. Research shows that the single-layer molybdenum disulfide has higher specific surface area and stronger adsorptivity to gas molecules, and the prepared gas sensor has high sensitivity.
Further, the preparation of the interdigital electrode on the vanadium-doped molybdenum disulfide layer comprises the following steps:
spin coating photoresist above the vanadium-doped molybdenum disulfide layer, and carrying out photoetching on the photoresist to obtain a mask plate;
etching the vanadium-doped molybdenum disulfide layer through a mask plate to obtain a vanadium-doped molybdenum disulfide layer with a certain shape;
and removing residual photoresist, heating gold (Au), platinum (Pt) or silver (Ag) by using a vacuum evaporation coating process, and evaporating and plating the gold (Au), the platinum (Pt) or the silver (Ag) to a vanadium-doped molybdenum disulfide layer to form the required interdigital electrode.
By adopting the scheme, the interdigital electrode is suitable for being prepared on a plurality of vanadium-doped molybdenum disulfide layers.
Further, the preparation of the interdigital electrode on the vanadium-doped molybdenum disulfide layer comprises the following steps:
before gold (Au) is evaporated, a layer of metallic titanium is firstly evaporated on a molybdenum disulfide layer doped with vanadium.
By adopting the scheme, the metal titanium (Ti) can increase the adhesiveness of gold (Au), platinum (Pt) and silver (Ag) and the vanadium-doped molybdenum disulfide layer.
Further, the method for improving the molybdenum disulfide gas sensor by adopting vanadium further comprises the following steps:
and the protection is carried out through the encapsulation of the box body.
By adopting the scheme, the sensor material is protected from collision.
Preferably, in the process of preparing the vanadium-doped molybdenum disulfide layer on the dielectric layer, the molar ratio of the vanadium chloride to the molybdenum trioxide is 3% -9%.
More preferably, in the process of preparing the vanadium-doped molybdenum disulfide layer on the dielectric layer, the molar ratio of the vanadium chloride to the molybdenum trioxide is 5%.
By adopting the scheme, the vanadium can be doped better, and the response time or recovery time is better.
The invention also provides sensing equipment which comprises a box body and a sensor prepared by the method for improving the molybdenum disulfide gas sensor by adopting vanadium, wherein the sensor is arranged in the box body.
By adopting the scheme, vanadium is utilized in the sensor to optimize the molybdenum disulfide layer, the reaction intensity of the sensor is improved, the recovery time is shortened, and the sensor is protected by the box body.
Further, the sensor comprises a substrate, a dielectric layer, an interdigital electrode and an interdigital electrode structure, wherein the substrate, the dielectric layer and the interdigital electrode are sequentially arranged and paved from bottom to top, and the interdigital electrode structure is formed by a molybdenum disulfide layer improved by vanadium.
By adopting the scheme, vanadium is utilized to optimize the molybdenum disulfide layer in the sensor, so that the reaction intensity of the sensor is improved, and the recovery time is shortened.
Further, the molybdenum disulfide of the molybdenum disulfide layer improved by vanadium is a single layer.
By adopting the scheme, the sensor can be prepared with less molybdenum disulfide layers such as a single layer, so that the sensor has higher sensitivity and wider applicability.
Further, the interdigital electrode structure is arranged in two forms, namely, the interdigital electrode is positioned above the molybdenum disulfide layer improved by vanadium, or the interdigital electrode is positioned below the molybdenum disulfide layer improved by vanadium.
By adopting the scheme, the interdigital electrode is prepared on a multi-layer vanadium-doped molybdenum disulfide layer or a few-layer vanadium-doped molybdenum disulfide layer.
In summary, the invention has the following beneficial effects:
1. the vanadium (V) is used for doping the molybdenum disulfide layer, so that adverse effects caused by molybdenum vacancies and sulfur vacancies are overcome, the reaction time of the sensor can be shortened, and the recovery time can be reduced;
2. the vanadium-doped molybdenum disulfide layer with a single layer and a few layers is obtained, so that the applicability of the sensor is improved;
3. the interdigital electrode structure is suitable for preparing interdigital electrodes on a multi-layer vanadium-doped molybdenum disulfide layer or a few-layer vanadium-doped molybdenum disulfide layer;
4. the sensor provided by the invention is simple to operate and convenient to carry;
5. the elastic cantilever is arranged around the inner wall of the lower box body of the sensor provided by the invention, and the elastic cantilever effectively replaces the prior art to place the sensor element in the shell in a fixed connecting piece or bonding mode. The elastic cantilever can be directly cut, punched and bent on a single metal aluminum sheet to be integrally formed, so that the manufacturing is convenient; the sensor element is clamped by means of deformation of the elastic cantilever, so that the assembly of the gas sensor is more convenient and quicker;
6. the disassembly connecting assembly provided by the invention effectively replaces the connection of the upper shell and the lower shell by using screws in the prior art, and solves the problems that the assembly or the disassembly is troublesome and the disassembly is inconvenient due to the fact that tools such as screwdrivers are needed to be used for assembly or disassembly during screw connection.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of one embodiment of a method of using vanadium to improve a molybdenum disulfide gas sensor in accordance with the present invention;
FIG. 2 is a flow chart of another embodiment of a method of using vanadium to improve a molybdenum disulfide gas sensor in accordance with the present invention;
FIG. 3 is an exploded view of one embodiment of the sensor of the present invention;
FIG. 4 is a perspective view of one embodiment of a sensor of the present invention;
FIG. 5 is a left side view of one embodiment of the sensor of the present invention;
FIG. 6 is a schematic view of one embodiment of a sensor element of the present invention;
FIG. 7 is a schematic view of one embodiment of a detachable connection assembly of the present invention;
FIG. 8 is a schematic view of an embodiment of a lower case of the present invention;
FIG. 9 is a schematic view of two embodiments of the connecting hole of the present invention;
FIG. 10 is a graph of the response of one embodiment of the sensor of the present invention to nitrogen dioxide;
FIG. 11 is a graph showing the response of one embodiment of the sensor of the present invention to ammonia gas;
description of the reference numerals
The technical scheme of the invention can be more clearly understood and described by the description of the reference numerals in combination with the embodiment of the invention.
The box body 1, the upper box body 11, the light source port 111, the vent hole 112, the first connecting hole 113, the lower box body 12, the elastic cantilever 121, the containing table 122, the second connecting hole 123, the clamping groove 1231, the notch 124 and the dismounting connecting component 13;
sensor 2, substrate 21, barrier layer 22, two-dimensional transition metal sulfide layer 23, jin Cha refer to electrode 24;
a flexible cantilever 121, a fixed segment 1211, a connecting segment 1212, a free end 1213;
the connection assembly 13, the chuck 131, the clamping boss 1311, the spring 132, the pressing plate 133, the connection post 134 and the handle 135 are disassembled.
Detailed Description
Reference will now be made in detail to exemplary embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, the same numbers in different drawings refer to the same or similar elements, unless otherwise indicated. The implementations described in the following exemplary examples do not represent all implementations consistent with the invention. Rather, they are merely examples of apparatus and methods consistent with aspects of the invention as detailed in the accompanying claims.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used in this specification and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It should also be understood that the term "and/or" as used herein refers to and encompasses any or all possible combinations of one or more of the associated listed items.
The present invention will be described in detail by examples.
Experimental example
Method one
A method for improving a molybdenum disulfide gas sensor using vanadium, comprising the steps of:
preparing 300-500 μm silicon as a substrate;
preparing silicon dioxide with the thickness of 200-300 mu m on a substrate by using a chemical deposition method as a dielectric layer;
weighing 0.08g of sulfur powder, 0.02g of molybdenum trioxide and vanadium chloride, mixing together, and then putting into a quartz boat;
covering a dielectric layer above the quartz boat;
putting the quartz boat into a single-temperature furnace, heating by setting parameters under the protection of hydrogen gas, wherein the heating temperature is 650 ℃, the heating time is 30min, and the heat preservation is 5min;
and naturally cooling to room temperature, taking out the quartz boat, and obtaining a vanadium-doped molybdenum disulfide layer on the dielectric layer.
Spin coating photoresist above the vanadium-doped molybdenum disulfide layer, and carrying out photoetching on the photoresist to obtain a mask plate;
etching the vanadium-doped molybdenum disulfide layer through a mask plate to obtain a vanadium-doped molybdenum disulfide layer with a certain shape;
and removing the residual photoresist, heating gold (Au) by utilizing a vacuum evaporation coating process, and evaporating to form a vanadium-doped molybdenum disulfide layer to form the required interdigital electrode.
The interdigital electrode is connected with the external pin.
Method II
Substantially the same as method one, except that: the gold vapor plating is changed into titanium vapor plating.
Method III
Substantially the same as method one, except that: before gold is evaporated, a layer of metallic titanium is evaporated on a molybdenum disulfide layer doped with vanadium.
Method IV
Substantially the same as method one, except that: sticking an adhesive tape on the vanadium-doped molybdenum disulfide layer, and tearing the adhesive tape, so that the molybdenum disulfide sheet layer is separated to obtain a thinner vanadium-doped molybdenum disulfide layer; repeating the steps; and detecting the number of layers of molybdenum disulfide by using a Raman spectrometer, and stopping repeating when a single layer is obtained.
Method five
Substantially the same as method one, except that: zinc chloride was used instead of vanadium chloride.
Method six
Substantially the same as method one, except that: and removing vanadium chloride.
Method seven
The method is the same as the method four, except that: and removing vanadium chloride.
Wherein the doping percentage is the mole ratio of doped metal atoms to molybdenum trioxide.
The grouping experiments were carried out with reference to the following table, 5ppm of NO was introduced 2, The response time of the reflected intensity was recorded and 5 replicates were run and averaged and the results are shown in the table below.
TABLE 1 influence of doping percentage and molybdenum disulfide layer number on sensor performance
By comparing the data in the table with the data in the group 1-5 and the group 14, the reaction intensity is improved, the reaction time is shortened, the recovery time is shortened (P < 0.01), and the performance of the molybdenum disulfide gas sensor can be greatly improved by adopting vanadium to improve the multi-layer molybdenum disulfide gas sensor; the comparison of the groups 1-5 with the groups 9-13 shows that the reaction intensity of the groups 2-4 is improved, the reaction time is shortened, the recovery time is obviously shortened (P is less than 0.01), and the molybdenum disulfide gas sensor doped with 3-9% of vanadium has better performance than the molybdenum disulfide gas sensor doped with 3-9% of zinc; group 7 has an increased reaction strength (P < 0.01) compared with groups 3 and 6, and the performance in reaction strength is better for the interdigitated electrodes of the two layers of titanium and gold in sequence than for the interdigitated electrode of the single layer of gold or titanium; the group 8 is compared with the group 15, the reaction intensity is improved, the reaction time is shortened, the recovery time is shortened (P < 0.01), and the performance of the molybdenum disulfide gas sensor can be greatly improved by adopting vanadium to improve the single-layer molybdenum disulfide gas sensor; compared with the group 3, the group 8 has the advantages that after vanadium doping is adopted, the reaction time of the single-layer molybdenum disulfide layer is shortened compared with that of the multi-layer molybdenum disulfide layer, and the recovery time is shortened (P < 0.01).
Examples
Referring to fig. 1, the present embodiment provides a method for improving a molybdenum disulfide gas sensor using vanadium, comprising the steps of:
s100, preparing a substrate;
s200, preparing a dielectric layer on a substrate by using a chemical deposition method;
s300, preparing a vanadium-doped molybdenum disulfide layer on the dielectric layer;
s400, preparing an interdigital electrode on a vanadium-doped molybdenum disulfide layer;
s500, connecting the interdigital electrode with an external pin.
The substrate can be silicon (Si), ceramic or the like, the dielectric layer can be silicon dioxide, aluminum oxide or the like, the interdigital electrode can be gold (Au), platinum (Pt), silver (Ag) or the like, and the external pin can be copper, aluminum or the like.
By adopting the scheme, the vanadium (V) is used for doping the molybdenum disulfide layer, so that adverse effects caused by molybdenum vacancies and sulfur vacancies are overcome, the reaction time of the sensor can be shortened, and the recovery time can be reduced.
Referring to fig. 2, in a preferred implementation of the present example, the preparing a vanadium doped molybdenum disulfide layer on the dielectric layer, comprises the steps of:
s311, weighing 0.08g of sulfur powder, 0.02g of molybdenum trioxide and vanadium chloride, mixing, and then putting into a quartz boat;
s312, covering a dielectric layer above the quartz boat;
s313, putting the quartz boat into a single-temperature furnace, and setting parameters for heating under the protection of hydrogen gas, wherein the heating temperature is T, the heating time is T1, and the heat preservation time is T2;
s314, naturally cooling to room temperature, taking out the quartz boat, and obtaining a vanadium-doped molybdenum disulfide layer on the dielectric layer.
By adopting the scheme, the molybdenum trioxide can be fully reduced under the action of hydrogen, vanadium is doped with molybdenum vacancies and sulfur vacancies, and the sensitivity of the sensor is improved.
In a preferred implementation of this example, the preparing a vanadium doped molybdenum disulfide layer on the dielectric layer includes preparing a monolayer of molybdenum disulfide using a mechanical lift-off process.
In a preferred implementation manner of this example, the step s300 of preparing a vanadium doped molybdenum disulfide layer on the dielectric layer includes the following steps:
s315, sticking an adhesive tape on the vanadium-doped molybdenum disulfide layer, and tearing the adhesive tape, so that the molybdenum disulfide sheet layer is separated to obtain a thinner vanadium-doped molybdenum disulfide layer;
s316, repeating the step S315;
s317, detecting the number of layers of molybdenum disulfide by using a Raman spectrometer, stopping repeating when a single vanadium-doped molybdenum disulfide layer is obtained, and detecting the number of layers of molybdenum disulfide by using other instruments, wherein the number of layers of molybdenum disulfide can be easily determined by a person skilled in the art.
Specifically, the raman spectrometer detection method can utilize a fingerprint vibration mode to analyze to obtain layer number information, and/or utilize a low wave number vibration mode to analyze to obtain layer number information.
By adopting the technical scheme, a single vanadium-doped molybdenum disulfide layer is obtained, and the applicability of the sensor is improved. Research shows that the single-layer molybdenum disulfide has higher specific surface area and stronger adsorptivity to gas molecules, and the prepared gas sensor has high sensitivity.
In a preferred implementation manner of this example, the preparation of the interdigital electrode on the vanadium doped molybdenum disulfide layer comprises the following steps:
s401, spin-coating photoresist above the vanadium-doped molybdenum disulfide layer, and carrying out photoetching on the photoresist to obtain a mask plate;
s402, etching the vanadium-doped molybdenum disulfide layer through a mask plate to obtain a vanadium-doped molybdenum disulfide layer with a certain shape; when the vanadium-doped molybdenum disulfide layer is a plurality of layers, etching can be performed or not, and when the vanadium-doped molybdenum disulfide layer is a single layer, the dielectric layer can be etched.
S404, removing residual photoresist, heating gold (Au), platinum (Pt) or silver (Ag) by using a vacuum evaporation coating process, and evaporating to form a vanadium-doped molybdenum disulfide layer to form the required interdigital electrode.
By adopting the scheme, the interdigital electrode is suitable for being prepared on a plurality of vanadium-doped molybdenum disulfide layers.
In a preferred implementation manner of this example, the preparation of the interdigital electrode on the vanadium doped molybdenum disulfide layer comprises the following steps:
s403, evaporating a layer of metallic titanium on the vanadium-doped molybdenum disulfide layer before evaporating gold. The underlayer will be formed as titanium. The upper layer is a gold double-layer interdigital electrode.
By adopting the scheme, the metal titanium (Ti) can increase the adhesiveness of gold (Au), platinum (Pt) and silver (Ag) and the vanadium-doped molybdenum disulfide layer.
In a preferred implementation of this embodiment, the method for improving a molybdenum disulfide gas sensor using vanadium further comprises the steps of:
s600, packaging and protecting through a box body.
By adopting the scheme, the sensor material is protected from collision.
TABLE 2 selection of materials, temperatures, times, etc. in different examples
Example IV
Referring to fig. 3 to 6, the present embodiment provides a sensing apparatus comprising a case 1 and a sensor 2 prepared by the above-described method for improving a molybdenum disulfide gas sensor using vanadium, the sensor 2 being disposed in the case 1.
By adopting the scheme, vanadium is utilized in the sensor 2 to optimize the molybdenum disulfide layer, the reaction intensity of the sensor 2 is improved, the recovery time is shortened, and the sensor 2 is protected by the box body 1.
In a preferred implementation of this embodiment, the sensor 2 includes a substrate 21, a dielectric layer 22, and an interdigital electrode structure formed by interdigital electrodes 24 and a molybdenum disulfide layer 23 modified with vanadium, which are sequentially arranged from bottom to top.
By adopting the scheme, vanadium is utilized in the sensor 2 to optimize the molybdenum disulfide layer, so that the reaction intensity of the sensor 2 is improved, and the recovery time is shortened.
In a preferred implementation of this example, the molybdenum disulfide of the molybdenum disulfide layer 23 is a single layer, which is modified with vanadium. The response curve for nitrogen dioxide at this time is shown in fig. 10, the response curve for ammonia is shown in fig. 11, and the detection limit for ammonia is detected to be less than 1.0ppm, and the detection limit for nitrogen dioxide is detected to be less than 0.8ppm.
By adopting the scheme, the sensor can be prepared with less molybdenum disulfide layers such as a single layer, so that the sensor has higher sensitivity and wider applicability.
In a preferred implementation of this embodiment, the interdigitated electrode structure is provided in two forms, i.e., the interdigitated electrode 24 is located above the molybdenum disulfide layer 23 modified with vanadium, or the interdigitated electrode 24 is located below the molybdenum disulfide layer 23 modified with vanadium.
By adopting the scheme, the interdigital electrode is prepared on the molybdenum disulfide layer 23 which is suitable for multiple layers of doped vanadium or the molybdenum disulfide layer 23 which is less in layers of doped vanadium.
In a preferred implementation of this embodiment, 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.
In a preferred implementation of this embodiment, the material of the dielectric layer 22 is silicon dioxide. In a preferred implementation of this embodiment, the dielectric layer 22 has a thickness of 200 μm to 300 μm.
In a preferred implementation of this embodiment, the case 1 includes an upper case 11 and a lower case 12, and the upper case 11 and the lower case 12 are connected by a detachable connection assembly 13.
In a preferred implementation manner of this embodiment, the upper case 11 is a rectangular aluminum alloy case, the top of the upper case is provided with a light source opening 111 for light source irradiation, and ventilation holes 112 are formed around the upper case 11, and the ventilation holes 112 are square holes, so that gas passing through can be detected conveniently. In addition, connecting tables are formed at four top corners of the upper box body 11, a first connecting hole 113 is formed on the connecting tables in a penetrating mode, and a guide groove is formed in the inner wall of the first connecting hole 113 along the axial direction and used for enabling the dismounting connecting assembly 13 to penetrate through.
The lower case 12 is a rectangular aluminum alloy case, which is adapted to the structure of the sensor 2. And the lower box 12 is provided with a hollow cavity for accommodating the sensor 2, the sensor 2 is arranged in the hollow cavity, and elastic cantilevers 121 are arranged around the hollow cavity. The present invention provides that the resilient cantilever 121 effectively replaces the prior art of positioning the sensor 2 within the housing by means of a fixed connection or adhesive. The elastic cantilever 121 can be directly cut, punched and bent on a single metal aluminum sheet to be integrally formed, so that the manufacturing is convenient; and the sensor 2 is clamped by means of deformation of the elastic cantilever 121, so that the assembly of the gas sensor is more convenient and quick.
Referring to fig. 8, in order to enable a person skilled in the art to better implement the technical solution of the present invention, describing the elastic cantilever 121 in detail, the elastic cantilever 121 includes a fixed section 1211, a connecting 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 2, and the connecting section 1212 is used for connecting the fixed section 1211 and the free end 1213. When the sensor 2 is installed in contact with the elastic cantilever 121, the free end 1213 approaches the fixed section 1211, the connecting section 1212 is correspondingly deformed to a certain extent, and when the sensor 2 is installed in the hollow cavity, the connecting section 1212 is restored to the original shape, and the free end 1213 is far away from the fixed section 1211 and clamps the sensor 2.
In a preferred implementation of this embodiment, the free end 1213 is recessed to form a fixing slot for accommodating the sensor 2, and by adopting this technical solution, the free end 1213 limits the sensor 2, so as to avoid the sensor 2 from sliding out of the free end 1213.
In a preferred implementation manner of this embodiment, a holding table 122 is disposed below the elastic cantilever 121 and located on the bottom surface of the hollow cavity, and the sensor 2 is supported by the holding table 122, so that a certain gap is formed between the sensor 2 and the bottom surface of the hollow cavity, and interference of the metal shell on the sensor 2 is avoided, and detection accuracy is affected. At the same time, the sensor 2 is better contacted with the elastic cantilever 121, so that the clamping of the sensor 2 in the lower box body 12 is more stable.
Referring to fig. 3, 8 and 9, in a preferred embodiment of the present embodiment, connection lugs are respectively disposed at four corners of the lower case 12, and the connection lugs are provided with connection holes two 123 corresponding to the connection holes one 113, and guide grooves are also formed on the inner walls of the connection holes two 123 in the axial direction. And upwards set up joint groove 1231 at the lower terminal surface of connecting hole two 123, this joint groove 1231 and guide way are perpendicular to be distributed on the lower terminal surface of connecting hole two 123, and its joint groove 1231 is less than the degree of depth of connecting hole two 123 along axial length, can realize dismantling the chucking spacing of coupling assembling 13. In addition, a notch 124 through which the electrode lead passes is formed in the bottom surface of the lower case 12.
Referring to fig. 7, in order to enable a person skilled in the art to better implement the technical scheme of the present invention, the above-mentioned disassembly connection assembly 13 is described in detail, and the disassembly connection assembly 13 is provided, so that the connection of the upper and lower shells by using screws in the prior art is effectively replaced, and the problems of troublesome installation and inconvenient disassembly caused by the need of installing or disassembling by using tools such as screwdrivers in the prior art are solved. The disassembly connecting assembly 13 designed by the technical scheme comprises a connecting column 134, a chuck 131, a spring 132 and a pressing plate 133, wherein the chuck 131 is sequentially arranged on the connecting column 134 from bottom to top, a clamping protrusion 1311 is outwards arranged on the chuck 131 in a protruding mode, the clamping disc 131 and the connecting column 134 are integrally arranged, the spring 132 and the pressing plate 133 are both sleeved on the connecting column 134, in addition, a handle 135 is fixedly connected to one end, far away from the chuck 131, of the connecting column 134, and the handle 135 is arranged on the connecting column 134 in an interference fit mode after the spring 132 and the pressing plate 133 are sleeved into the connecting column 134.
Through adopting above-mentioned technical scheme, when last box body 11 and lower box body 12 are connected, with connecting hole one 113 and connecting hole two 123 alignment for card protruding 1311 aligns the guide slot and inserts, when spliced pole 134 carried chuck 131 to insert to the lower terminal surface of connecting hole two 123, spring 132 received extrusion shrink, and twist grip 135 makes card protruding 1311 keep away from the tip of guide slot, and gets into joint groove 1231, and spring 132 is in compressed state all the time, makes card protruding 1311 be located joint groove 1231 all the time, thereby makes convenient and difficult not hard up of connection. The diameter of the pressing plate 133 is larger than that of the first connecting hole 113, one end of the spring 132 is abutted to the pressing plate 133, and the pressing plate 133 is tightly attached to the upper end face of the first connecting hole 113.
In a preferred embodiment of the present embodiment, the guide groove and the locking groove 1231 are dovetail grooves, and the locking protrusion 1311 is a dovetail block, so that the contact area between the locking protrusion 1311 and the locking groove 1231 is increased, and the locking is more secure.
In a preferred implementation manner of this embodiment, an elastic member is disposed on the lower end surface of the pressing plate 133, so as to play a role of buffering; the upper end face of the pressing plate 133 is provided with a boss, a certain gap is reserved between the handle 135 and the pressing plate 133, and the handle 135 can be conveniently held for operation.
In a preferred implementation of this embodiment, the interdigital electrode structure is arranged in two forms, i.e. the interdigital electrode 24 is located above the vanadium-doped molybdenum disulfide layer 23 to form the surface sensor 2, or the interdigital electrode 24 is located below the vanadium-doped molybdenum disulfide layer 23 to form the intermediate sensor 2.
It should be noted that it will be apparent to those skilled in the art that various changes and modifications can be made to the present invention without departing from the principles of the invention, and such changes and modifications will fall within the scope of the appended claims.
Claims (7)
1. A method for improving a molybdenum disulfide gas sensor by using vanadium, which is characterized by comprising the following steps:
preparing a substrate;
preparing a dielectric layer on a substrate by using a chemical deposition method;
preparing a vanadium-doped molybdenum disulfide layer on the dielectric layer;
the method specifically comprises the following steps:
weighing quantitative sulfur powder, molybdenum trioxide and vanadium chloride, and then placing the materials into a quartz boat;
the molar ratio of the vanadium chloride to the molybdenum trioxide is 3% -9%;
covering a dielectric layer above the quartz boat;
putting the quartz boat into a single-temperature furnace, heating at 650 ℃ for 30-40 min under the protection of hydrogen gas, and preserving the temperature for 5-10 min;
naturally cooling to room temperature, taking out the quartz boat, and obtaining a vanadium-doped molybdenum disulfide layer on the dielectric layer;
preparing an interdigital electrode on the vanadium-doped molybdenum disulfide layer;
the method specifically comprises the following steps:
spin coating photoresist above the vanadium-doped molybdenum disulfide layer, and carrying out photoetching on the photoresist to obtain a mask plate;
etching the vanadium-doped molybdenum disulfide layer through a mask plate to obtain a vanadium-doped molybdenum disulfide layer with a certain shape;
removing residual photoresist, heating gold (Au), platinum (Pt) or silver (Ag) by using a vacuum evaporation coating process, evaporating to form a vanadium-doped molybdenum disulfide layer, and forming a required interdigital electrode;
the interdigital electrode is connected with the external pin.
2. The method of claim 1, wherein preparing a vanadium doped molybdenum disulfide layer on the dielectric layer comprises preparing a single layer of molybdenum disulfide by mechanical lift-off.
3. The method for improving a molybdenum disulfide gas sensor using vanadium according to claim 2, wherein the method for preparing a vanadium doped molybdenum disulfide layer on the dielectric layer comprises the steps of:
sticking an adhesive tape on the vanadium-doped molybdenum disulfide layer, and tearing the adhesive tape, so that the molybdenum disulfide sheet layer is separated to obtain a thinner vanadium-doped molybdenum disulfide layer;
repeating the steps;
and detecting the number of layers of molybdenum disulfide by using an instrument, and stopping repeating when a single vanadium-doped molybdenum disulfide layer is obtained.
4. The method for improving a molybdenum disulfide gas sensor using vanadium according to claim 3, wherein the preparing an interdigital electrode on the vanadium doped molybdenum disulfide layer comprises the steps of:
before gold is evaporated, a layer of metallic titanium is evaporated on a molybdenum disulfide layer doped with vanadium.
5. The method for improving a molybdenum disulfide gas sensor by using vanadium according to claim 1, wherein in the process of preparing a vanadium-doped molybdenum disulfide layer on the dielectric layer, the molar ratio of vanadium chloride to molybdenum trioxide is 5%.
6. A sensing device, characterized by comprising a cartridge (1) and a sensor (2) prepared by the method of any one of claims 1-5 using vanadium to improve a molybdenum disulfide gas sensor, the sensor (2) being disposed within the cartridge (1); the box body (1) comprises an upper box body (11) and a lower box body (12), and the upper box body (11) and the lower box body (12) are connected through a disassembly connecting assembly (13); the lower box body (12) is provided with a hollow cavity for accommodating the sensor (2), the sensor (2) is arranged in the hollow cavity, and elastic cantilevers (121) are arranged around the hollow cavity.
7. The sensing device according to claim 6, wherein the sensor (2) comprises a substrate (21), a dielectric layer (22), and an interdigital electrode structure of interdigital electrodes (24) and molybdenum disulfide layer shapes (23) improved by vanadium, which are sequentially arranged from bottom to top.
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