CN108169284A - Humidity sensor based on carbon dots doping molybdenum disulfide thin slice and preparation method thereof - Google Patents
Humidity sensor based on carbon dots doping molybdenum disulfide thin slice and preparation method thereof Download PDFInfo
- Publication number
- CN108169284A CN108169284A CN201711339515.4A CN201711339515A CN108169284A CN 108169284 A CN108169284 A CN 108169284A CN 201711339515 A CN201711339515 A CN 201711339515A CN 108169284 A CN108169284 A CN 108169284A
- Authority
- CN
- China
- Prior art keywords
- molybdenum disulfide
- carbon
- carbon dot
- doped molybdenum
- compound
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 85
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title abstract description 10
- 150000001875 compounds Chemical class 0.000 claims abstract description 45
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 108
- 229910052799 carbon Inorganic materials 0.000 claims description 108
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 52
- 239000003153 chemical reaction reagent Substances 0.000 claims description 31
- 239000007864 aqueous solution Substances 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 14
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 13
- 229910052750 molybdenum Inorganic materials 0.000 claims description 13
- 239000011733 molybdenum Substances 0.000 claims description 13
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 claims description 12
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 11
- 229910052717 sulfur Inorganic materials 0.000 claims description 11
- 239000011593 sulfur Substances 0.000 claims description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- -1 molybdenum disulfide compound Chemical class 0.000 claims description 9
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- 229960002989 glutamic acid Drugs 0.000 claims description 6
- 238000012544 monitoring process Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- RHGKLRLOHDJJDR-BYPYZUCNSA-N L-citrulline Chemical compound NC(=O)NCCC[C@H]([NH3+])C([O-])=O RHGKLRLOHDJJDR-BYPYZUCNSA-N 0.000 claims description 3
- KDXKERNSBIXSRK-YFKPBYRVSA-N L-lysine Chemical compound NCCCC[C@H](N)C(O)=O KDXKERNSBIXSRK-YFKPBYRVSA-N 0.000 claims description 3
- QIVBCDIJIAJPQS-VIFPVBQESA-N L-tryptophane Chemical compound C1=CC=C2C(C[C@H](N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-VIFPVBQESA-N 0.000 claims description 3
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004472 Lysine Substances 0.000 claims description 3
- RHGKLRLOHDJJDR-UHFFFAOYSA-N Ndelta-carbamoyl-DL-ornithine Natural products OC(=O)C(N)CCCNC(N)=O RHGKLRLOHDJJDR-UHFFFAOYSA-N 0.000 claims description 3
- QIVBCDIJIAJPQS-UHFFFAOYSA-N Tryptophan Natural products C1=CC=C2C(CC(N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-UHFFFAOYSA-N 0.000 claims description 3
- 239000012378 ammonium molybdate tetrahydrate Substances 0.000 claims description 3
- FIXLYHHVMHXSCP-UHFFFAOYSA-H azane;dihydroxy(dioxo)molybdenum;trioxomolybdenum;tetrahydrate Chemical compound N.N.N.N.N.N.O.O.O.O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O FIXLYHHVMHXSCP-UHFFFAOYSA-H 0.000 claims description 3
- 235000013477 citrulline Nutrition 0.000 claims description 3
- 229960002173 citrulline Drugs 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 3
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 claims description 3
- 235000018417 cysteine Nutrition 0.000 claims description 3
- 229960002433 cysteine Drugs 0.000 claims description 3
- 229960003646 lysine Drugs 0.000 claims description 3
- 239000012046 mixed solvent Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 3
- RWVGQQGBQSJDQV-UHFFFAOYSA-M sodium;3-[[4-[(e)-[4-(4-ethoxyanilino)phenyl]-[4-[ethyl-[(3-sulfonatophenyl)methyl]azaniumylidene]-2-methylcyclohexa-2,5-dien-1-ylidene]methyl]-n-ethyl-3-methylanilino]methyl]benzenesulfonate Chemical compound [Na+].C1=CC(OCC)=CC=C1NC1=CC=C(C(=C2C(=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=2C(=CC(=CC=2)N(CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=C1 RWVGQQGBQSJDQV-UHFFFAOYSA-M 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 3
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 3
- 229960004799 tryptophan Drugs 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- 239000002135 nanosheet Substances 0.000 claims 2
- 230000035945 sensitivity Effects 0.000 abstract description 5
- 239000002060 nanoflake Substances 0.000 abstract description 2
- 239000011888 foil Substances 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 description 14
- 238000001514 detection method Methods 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 230000007547 defect Effects 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000012043 crude product Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 235000015393 sodium molybdate Nutrition 0.000 description 3
- 239000011684 sodium molybdate Substances 0.000 description 3
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000012265 solid product Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000011540 sensing material Substances 0.000 description 2
- 235000013878 L-cysteine Nutrition 0.000 description 1
- 239000004201 L-cysteine Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920005597 polymer membrane Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000758 substrate 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
Landscapes
- Chemical & Material Sciences (AREA)
- 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 kind of compound based on carbon dots doping molybdenum disulfide thin slice, wherein, the compound of carbon dots doping molybdenum disulfide thin slice is two-dimensional nano flake.The present invention also provides the preparation method and its usages of the compound based on carbon dots doping molybdenum disulfide thin slice.The present invention also provides the humidity sensor for including the compound based on carbon dots doping molybdenum disulfide thin slice, preparation method and the usages.The compound based on carbon dots doping molybdenum disulfide thin slice prepared by the present invention and the humidity sensor based on carbon dots doping molybdenum disulfide foil laminates have wider response range and show linear response, fast response time, high sensitivity, Repeatability are excellent.
Description
Technical Field
The invention relates to the technical field of gas sensing, in particular to a humidity sensor based on a carbon point doped and modified molybdenum disulfide sheet and a preparation method thereof.
Background
Humidity is an important parameter for environmental assessment because it is inseparably linked to many things in the environment. In addition to this, humidity has a considerable influence on industrial production and technical development. The measurement and continuous monitoring of humidity are important in many fields such as semiconductor manufacturing, packaging industry, soil moisture monitoring, pharmaceutical and food processing, civil engineering, electronic processing, household appliances and air conditioning systems. A recent survey shows that the market share of humidity sensors is expected to reach $ 23 billion by 2020. Therefore, the humidity sensor which is developed and researched and has the advantages of quick response, high sensitivity, wide test range and low cost is an urgent need for the development of the current society.
The humidity sensing materials in the most commercially available humidity sensors at present are porous ceramic and polymer membranes. The polymer sensing material has the defects of incapability of running under a high humidity level, display lag, slow response, easy loss for a long time and the like. Commercial humidity sensors also use metal oxides as the sensing layer, with the disadvantage of requiring periodic thermal cleaning to restore their humidity sensing characteristics. In addition, hydroxyl ions are gradually chemically adsorbed on the surface of the sensing layer, so that the resistance of the sensing layer is gradually changed, and the humidity sensing performance of the sensing layer is reduced. At present, many research groups are dedicated to develop high-performance humidity sensing nano materials, such as nano silicon, nano ceramic, semiconductor nano particles, metal oxide nano wires and the like, and the practical application has the defects of high cost, difficulty in realizing wide application and the like.
In the prior art, the two-dimensional metal sulfide molybdenum disulfide with a graphene-like structure has great potential in the field of gas sensing due to the advantages of large specific surface area, high electron mobility and conductivity, low background noise and the like. However, the substrate surface of the two-dimensional molybdenum disulfide is catalytically inert, the active site is only located at the edge of the layer, and the original molybdenum disulfide surface has no active functional group, which results in very limited absorption amount of molybdenum disulfide to water molecules, so that electron transfer between molybdenum disulfide and water molecules cannot be continuously performed in actual use, and finally, the sensing defect that the humidity sensor based on molybdenum disulfide shows low sensitivity and long response time is caused.
Accordingly, those skilled in the art have endeavored to develop a humidity sensor based on carbon dot-doped molybdenum disulfide flakes and a method for making the same.
Disclosure of Invention
In view of the above defects in the prior art, the technical problems to be solved by the present invention are that the existing molybdenum disulfide degree sensor has low sensitivity to humidity response and long response time.
In order to achieve the above object, the present invention provides a composite based on carbon dot-doped molybdenum disulfide flakes;
wherein the compound of the carbon dot doped molybdenum disulfide flake is in a two-dimensional nanometer flake shape.
The invention also provides a humidity sensor based on the carbon dot doped molybdenum disulfide sheet, which comprises a compound of the carbon dot doped molybdenum disulfide sheet as a humidity sensing layer.
The invention also provides a preparation method of the carbon dot doped molybdenum disulfide flake-based compound, which comprises the following steps:
step 1, adding a carbon source into water to prepare a carbon dot aqueous solution;
and 2, adding a molybdenum source reagent and a sulfur source reagent into the carbon dot aqueous solution obtained in the step 1, and preparing and post-treating the mixture by adopting a one-step hydrothermal method to obtain the carbon dot doped molybdenum disulfide flake compound.
The invention also provides a preparation method of the humidity sensor based on the carbon point doped molybdenum disulfide sheet, which comprises the steps of the preparation method of the compound based on the carbon point doped molybdenum disulfide sheet and the following steps:
and 3, mixing the carbon point doped molybdenum disulfide compound obtained in the step 2 with an alcohol reagent, dropwise adding the mixture onto the interdigital electrode, and drying to obtain the humidity sensor of the carbon point doped molybdenum disulfide sheet.
Further, in the step 1, a method for preparing the carbon dot aqueous solution is selected from one of a microwave method, a hydrothermal method and a high-temperature melting method;
further, in the step 1, the carbon source is selected from one or more of L-glutamic acid, cysteine, lysine, tryptophan and citrulline;
further, in the step 1, the weight-to-volume ratio (mg/ml) of the carbon source to the water is 10: 1-20: 1;
further, in the step 2, the molybdenum source reagent is selected from one or more of sodium molybdate dihydrate and ammonium molybdate tetrahydrate;
further, in the step 2, the sulfur source reagent is selected from one or more of thiourea and thioacetamide;
further, in the step 2, the weight-to-volume ratio (mg/ml) of the molybdenum source reagent to the carbon dot aqueous solution is 20: 1-40: 1;
further, in the step 2, the weight-to-volume ratio (mg/ml) of the sulfur source reagent to the carbon dot aqueous solution is 10: 1-20: 1; preferably 13: 1;
further, in the step 2, the reaction temperature of the one-step hydrothermal method is 160-240 ℃, and the reaction time is 12-36 hours;
further, in the step 2, the post-treatment comprises washing and centrifuging;
further, the washed solvent is selected from one of water, ethanol or a mixed solvent of water and ethanol; the centrifugal speed is 5000-10000 rpm, and the centrifugal time is 5-30 min;
further, in the step 3, the alcohol reagent is selected from one or more of methanol, ethanol, propanol and butanol;
further, in the step 3, the dropwise adding volume of the carbon dot doped molybdenum disulfide compound alcohol mixed solution is 1-5 μ L;
further, in the step 3, the drying temperature is 50-100 ℃, and the drying time is 0.5-3 h.
In a preferred embodiment of the present invention, in step 1, the method for preparing the aqueous solution of carbon dots is a hydrothermal method; wherein the reaction temperature of the hydrothermal method is 200 ℃, and the reaction time is 12 h;
in another preferred embodiment of the present invention, in the step 1, the method for preparing the aqueous solution of carbon dots is a high temperature melting method; wherein the reaction temperature of the high-temperature melting method is 250 ℃;
in another preferred embodiment of the present invention, in the step 1, the method for preparing the aqueous solution of carbon dots is a microwave method; wherein the microwave reaction temperature is 200 ℃, and the microwave reaction time is 30 min;
in another preferred embodiment of the present invention, in the step 1, the weight/volume ratio (mg/ml) of the carbon source to the water is 10: 1;
in another preferred embodiment of the present invention, in the step 1, the weight/volume ratio (mg/ml) of the carbon source to the water is 20: 1;
in another preferred embodiment of the present invention, in the step 1, the weight/volume ratio (mg/ml) of the carbon source to the water is 13: 1;
in another preferred embodiment of the present invention, in the step 2, the weight/volume ratio (mg/ml) of the molybdenum source reagent to the carbon dot aqueous solution is 20: 1;
in another preferred embodiment of the present invention, in the step 2, the weight/volume ratio (mg/ml) of the molybdenum source reagent to the carbon dot aqueous solution is 30: 1;
in another preferred embodiment of the present invention, in the step 2, the weight/volume ratio (mg/ml) of the molybdenum source reagent to the carbon dot aqueous solution is 40: 1;
in another preferred embodiment of the present invention, in the step 2, the weight/volume ratio (mg/ml) of the sulfur source reagent to the carbon dot aqueous solution is 13: 1;
in another preferred embodiment of the present invention, in the step 2, the reaction temperature of the one-step hydrothermal method is 200 ℃, and the reaction time is 24 hours;
in another preferred embodiment of the present invention, in the step 3, the alcohol reagent is ethanol;
in another preferred embodiment of the present invention, in the step 3, the drying temperature is 60 ℃ and the drying time is 0.5 h.
The invention also provides a compound based on the carbon dot doped molybdenum disulfide flake, and an application of the compound based on the carbon dot doped molybdenum disulfide flake prepared by any preparation method in preparation of a compound for humidity sensing monitoring.
The invention also provides a humidity sensor based on the carbon point doped molybdenum disulfide sheet, and application of the humidity sensor based on the carbon point doped molybdenum disulfide sheet prepared by any preparation method in preparation of humidity sensing monitoring.
By adopting the scheme, the carbon-point-doped molybdenum disulfide flake-based compound, the humidity sensor and the preparation method disclosed by the invention have the following advantages:
the preparation process of the carbon-point-doped molybdenum disulfide flake-based compound is simple, the raw materials are wide in source and low in cost, and industrial production and application are easy to realize;
the carbon point doped molybdenum disulfide flake-based compound and the humidity sensor prepared from the compound have the advantages that the response sensitivity to humidity in the environment is high at room temperature, the response speed is high, the linear response is shown in a certain measurement range, and the humidity sensor has excellent humidity response performance;
compared with the existing humidity sensing nano material, the carbon-point-doped molybdenum disulfide flake-based compound has the advantages of low preparation cost, environmental friendliness, capability of reducing the use cost to the maximum extent in practical application, wide application in various humidity monitoring fields and great application prospect.
The conception, the specific technical solutions and the technical effects produced by the present invention will be further described with reference to the preferred embodiments so that the objects, the features and the effects of the present invention can be fully understood.
Drawings
Figure 1 is a scanning electron microscope image of a composite based on carbon dot doped molybdenum disulfide flakes of example 1;
FIG. 2 is a graph of the humidity response repeatability of the humidity sensor based on carbon dot doped molybdenum disulfide flakes of example 1 at 75% relative humidity;
FIG. 3 is a graph showing the response of a humidity sensor based on carbon dot doped molybdenum disulfide flakes to humidity detection at different humidities in example 1;
FIG. 4 is a linear fit of the humidity sensor based on carbon dot doped molybdenum disulfide flakes of example 1 to the humidity detection response at different humidities.
Detailed Description
The following describes several preferred embodiments of the present invention to make the technical contents thereof clearer and easier to understand. The invention may be embodied in many different forms of embodiments, which are intended to be illustrative only, and the scope of the invention is not intended to be limited to the embodiments shown herein.
If there is an experimental method not specified specific conditions, it is usually carried out according to conventional conditions, such as the relevant instructions or manuals.
Example 1 preparation of a Compound based on carbon dot-doped molybdenum disulfide flakes and humidity sensor
Step 1, adding 300mg of L-glutamic acid into 30mL of water, uniformly dispersing, transferring into a reaction kettle, heating at 200 ℃ for 12 hours, and cooling to obtain a carbon dot aqueous solution;
and 2, adding 900mg of sodium molybdate and 390mg of thiourea into the 30mL of carbon dot aqueous solution obtained in the step 1, dispersing to obtain a uniform solution, and transferring to a reaction kettle. Heating for 24 hours at 200 ℃ to obtain a crude solid product of the carbon-point-doped molybdenum disulfide compound;
washing the solid crude product with deionized water and ethanol alternately for 3 times respectively, and centrifuging at the centrifugal speed of 7000rpm for 10min to obtain a compound based on the carbon dot doped molybdenum disulfide flake;
and 3, dissolving the compound based on the carbon point doped molybdenum disulfide flake obtained in the step 2 in absolute ethyl alcohol, measuring 2 mu L of the compound by a liquid transfer gun, dropwise adding the compound onto the interdigital electrode, and drying the electrode in an oven at 60 ℃ for 0.5h after the ethyl alcohol is completely volatilized to obtain the humidity sensor based on the carbon point doped molybdenum disulfide flake.
Scanning the compound based on the carbon dot doped molybdenum disulfide flake obtained in the step 2 by an electron microscope, as shown in fig. 1, the compound based on the carbon dot doped molybdenum disulfide flake of the embodiment has a uniform morphology and is composed of two-dimensional nano flakes.
Example 2 preparation of a Compound based on carbon dot-doped molybdenum disulfide flakes and humidity sensor
Step 1, adding 1200mg of L-glutamic acid into a round-bottom flask, heating to 250 ℃ until the L-glutamic acid is melted into a tawny liquid, adding 90mL of deionized water, dissolving, and centrifuging to remove large particles to obtain a carbon dot aqueous solution;
and 2, adding 600mg of sodium molybdate and 390mg of thiourea into the 30mL of carbon dot aqueous solution obtained in the step 1, dispersing to obtain a uniform solution, and transferring to a reaction kettle. Heating at 160 ℃ for 36h to obtain a crude solid product of the carbon-point-doped molybdenum disulfide compound;
and (3) alternately washing the solid crude product with deionized water and ethanol for 3 times respectively, and centrifuging for 30min at the centrifugal speed of 5000rpm to obtain the compound based on the carbon point doped molybdenum disulfide flake.
And 3, dissolving the compound based on the carbon point doped molybdenum disulfide flake obtained in the step 2 in absolute ethyl alcohol, measuring 2 mu L of the compound by a liquid transfer gun, dropwise adding the compound onto the interdigital electrode, and drying the electrode in an oven at 80 ℃ for 3h after the ethyl alcohol is completely volatilized to obtain the humidity sensor based on the carbon point doped molybdenum disulfide flake.
Example 3 preparation of a Compound based on carbon dot-doped molybdenum disulfide flakes and humidity sensor
Step 1, adding 300mg of L-cysteine into 15mL of water, uniformly dispersing, transferring into a microwave reaction bottle, and carrying out microwave reaction at 200 ℃ for 30min to obtain a carbon dot aqueous solution;
and 2, adding 1200mg of sodium molybdate and 390mg of thiourea into the 30mL of carbon dot aqueous solution obtained in the step 1, dispersing to obtain a uniform solution, and transferring to a reaction kettle. Heating at 240 ℃ for 12h to obtain a crude solid product of the carbon-point-doped molybdenum disulfide compound;
and (3) alternately washing the solid crude product with deionized water and ethanol for 3 times respectively, and centrifuging at the centrifugal speed of 8000rpm for 8min to obtain the compound based on the carbon point doped molybdenum disulfide flake.
And 3, dissolving the compound based on the carbon point doped molybdenum disulfide flake obtained in the step 2 in absolute ethyl alcohol, measuring 2 mu L of the compound by a liquid transfer gun, dropwise adding the compound onto the interdigital electrode, and drying the electrode in an oven at 100 ℃ for 0.5h after the ethyl alcohol is completely volatilized to obtain the humidity sensor based on the carbon point doped molybdenum disulfide flake.
Test example 4 humidity response test
(1) Example 1 a humidity sensor based on carbon dot doped molybdenum disulfide flakes performs repeated humidity response measurements at 75% relative humidity;
as shown in fig. 2, the detection response curves of the humidity sensor based on the carbon dot-doped molybdenum disulfide flake in example 1 of the present invention after repeating 4 times within 2000 seconds at 75% relative humidity are substantially consistent, and the humidity sensor shows fast response and good repeatability, which indicates that the humidity sensor based on the carbon dot-doped molybdenum disulfide flake in example 1 of the present invention has excellent response and repeatability.
(2) Example 1 a humidity sensor based on carbon dot doped molybdenum disulfide flakes performs humidity response detection at different humidities;
as shown in fig. 3, the humidity sensor based on the carbon dot-doped molybdenum disulfide flake in embodiment 1 of the present invention all shows a strong response signal at 15% to 80% relative humidity, which indicates that the humidity sensor based on the carbon dot-doped molybdenum disulfide flake in embodiment 1 of the present invention has a wide response range and can be widely applied to various detection environments with different humidities.
The response values of the humidity sensor based on the carbon point doped molybdenum disulfide flake in the embodiment 1 for humidity response detection under different humidities are subjected to linear fitting, and the result is shown in fig. 4, wherein the humidity sensor based on the carbon point doped molybdenum disulfide flake in the embodiment 1 of the invention presents linear response under 15% -80% relative humidity; the humidity sensor based on the carbon dot doped molybdenum disulfide flake in the embodiment 1 of the invention has excellent humidity detection performance.
In summary, the humidity sensor based on the carbon dot doped molybdenum disulfide flake according to the embodiment of the present invention has excellent humidity sensing response repeatability, has a wide response range, and exhibits linear response, which indicates that the humidity sensor based on the carbon dot doped molybdenum disulfide flake according to the embodiment of the present invention has excellent performance in various aspects of humidity detection.
The technical scheme of other embodiments of the invention also has similar beneficial effects as described above.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (10)
1. The compound based on the carbon dot doped molybdenum disulfide flake is characterized in that the compound based on the carbon dot doped molybdenum disulfide flake is in a two-dimensional nanosheet shape.
2. A humidity sensor based on carbon dot doped molybdenum disulfide flakes, comprising the compound based on carbon dot doped molybdenum disulfide flakes of claim 1 as a humidity sensing layer.
3. A preparation method of a compound based on carbon dot doped molybdenum disulfide flakes is characterized by comprising the following steps:
step 1, adding a carbon source into water to prepare a carbon dot aqueous solution;
and 2, adding a molybdenum source reagent and a sulfur source reagent into the carbon dot aqueous solution obtained in the step 1, and preparing and post-treating the mixture by adopting a one-step hydrothermal method to obtain the carbon dot doped molybdenum disulfide flake compound.
4. A method for preparing a humidity sensor based on a carbon dot doped molybdenum disulfide sheet is characterized by comprising the following steps:
step 1, adding a carbon source into water to prepare a carbon dot aqueous solution;
step 2, adding a molybdenum source reagent and a sulfur source reagent into the carbon dot aqueous solution obtained in the step 1, and preparing and post-treating the mixture by adopting a one-step hydrothermal method to obtain a carbon dot doped molybdenum disulfide sheet compound;
and 3, mixing the carbon point doped molybdenum disulfide compound obtained in the step 2 with an alcohol reagent, dropwise adding the mixture onto the interdigital electrode, and drying to obtain the humidity sensor of the carbon point doped molybdenum disulfide sheet.
5. The method according to claim 3 or 4, wherein,
in the step 1, the method for preparing the carbon dot aqueous solution is selected from one of a microwave method, a hydrothermal method and a high-temperature melting method;
in the step 1, the carbon source is selected from one or more of L-glutamic acid, cysteine, lysine, tryptophan and citrulline;
in the step 1, the weight volume ratio of the carbon source to the water is 10: 1-30: 1.
6. The method according to claim 3 or 4, wherein,
in the step 2, the molybdenum source reagent is selected from one or more of sodium molybdate dihydrate and ammonium molybdate tetrahydrate;
in the step 2, the sulfur source reagent is selected from one or more of thiourea and thioacetamide;
in the step 2, the weight volume ratio of the molybdenum source reagent to the carbon dot aqueous solution is 20: 1-40: 1;
in the step 2, the weight volume ratio of the sulfur source reagent to the carbon dot aqueous solution is 10: 1-20: 1;
in the step 2, the reaction temperature of the one-step hydrothermal method is 160-240 ℃, and the reaction time is 12-36 hours;
in the step 2, the post-treatment comprises washing and centrifuging; the washed solvent is selected from one of water and ethanol or a mixed solvent of water and ethanol; the centrifugal speed is 5000-10000 rpm, and the centrifugal time is 5-30 min.
7. The method according to claim 3 or 4, wherein,
in the step 3, the alcohol reagent is selected from one or more of methanol, ethanol, propanol and butanol;
in the step 3, the dropping volume of the carbon dot doped molybdenum disulfide compound and the alcohol mixture is 1-5 mu L;
in the step 3, the drying temperature is 50-100 ℃, and the drying time is 0.5-3 h.
8. The compound based on the carbon dot doped molybdenum disulfide flake obtained by the preparation method of claim 3, wherein the compound based on the carbon dot doped molybdenum disulfide flake is a two-dimensional nanosheet.
9. The humidity sensor based on the carbon dot doped molybdenum disulfide flake obtained by the preparation method of claim 4, which is characterized by comprising the following steps:
step 1, adding a carbon source into water to prepare a carbon dot aqueous solution;
step 2, adding a molybdenum source reagent and a sulfur source reagent into the carbon dot aqueous solution obtained in the step 1, and preparing and post-treating the mixture by adopting a one-step hydrothermal method to obtain a carbon dot doped molybdenum disulfide sheet compound;
step 3, mixing the carbon point doped molybdenum disulfide compound obtained in the step 2 with an alcohol reagent, dropwise adding the mixture onto an interdigital electrode, and drying to obtain a humidity sensor of the carbon point doped molybdenum disulfide sheet;
wherein,
in the step 1, the method for preparing the carbon dot aqueous solution is selected from one of a microwave method, a hydrothermal method and a high-temperature melting method;
in the step 1, the carbon dot raw material is selected from one or more of L-glutamic acid, cysteine, lysine, tryptophan and citrulline;
in the step 1, the weight volume ratio of the carbon source to the water is 10: 1-30: 1;
in the step 2, the molybdenum source reagent is selected from one or more of sodium molybdate dihydrate and ammonium molybdate tetrahydrate;
in the step 2, the sulfur source reagent is selected from one or more of thiourea and thioacetamide;
in the step 2, the weight volume ratio of the molybdenum source reagent to the carbon dot aqueous solution is 20: 1-40: 1;
in the step 2, the weight volume ratio of the sulfur source reagent to the carbon dot aqueous solution is 10: 1-20: 1;
in the step 2, the reaction temperature of the one-step hydrothermal method is 160-240 ℃, and the reaction time is 12-36 hours;
in the step 2, the post-treatment comprises washing and centrifuging; the washed solvent is selected from one of water and ethanol or a mixed solvent of water and ethanol; the centrifugal speed is 5000-10000 rpm, and the centrifugal time is 5-30 min;
in the step 3, the alcohol reagent is selected from one or more of methanol, ethanol, propanol and butanol;
in the step 3, the dropping volume of the carbon dot doped molybdenum disulfide compound and the alcohol mixture is 1-5 mu L;
in the step 3, the drying temperature is 50-100 ℃, and the drying time is 0.5-3 h.
10. Use of a composite based on carbon dot doped molybdenum disulphide flakes according to any one of claims 1 and 8, or a humidity sensor based on carbon dot doped molybdenum disulphide flakes according to any one of claims 2 and 9, for the preparation of a humidity sensor for monitoring.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711339515.4A CN108169284B (en) | 2017-12-14 | 2017-12-14 | Humidity sensor based on carbon dot doped molybdenum disulfide sheet and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711339515.4A CN108169284B (en) | 2017-12-14 | 2017-12-14 | Humidity sensor based on carbon dot doped molybdenum disulfide sheet and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108169284A true CN108169284A (en) | 2018-06-15 |
| CN108169284B CN108169284B (en) | 2021-01-01 |
Family
ID=62525355
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711339515.4A Active CN108169284B (en) | 2017-12-14 | 2017-12-14 | Humidity sensor based on carbon dot doped molybdenum disulfide sheet and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108169284B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108786857A (en) * | 2018-07-06 | 2018-11-13 | 中北大学 | A kind of carbon dots/two dimension MoS2Composite photo-catalyst and preparation method thereof |
| CN110208337A (en) * | 2019-06-28 | 2019-09-06 | 西南交通大学 | Compound humidity sensor of molybdenum disulfide/Nano diamond and preparation method thereof |
| CN110228821A (en) * | 2019-07-12 | 2019-09-13 | 安徽大学 | A kind of preparation method that carbon dots doping induces 1T phase molybdenum disulfide and the application in energy storage material |
| CN113029239A (en) * | 2021-03-11 | 2021-06-25 | 昆山联鲸仪智能科技有限公司 | Multifunctional sensor and preparation method thereof |
| CN113125520A (en) * | 2021-04-21 | 2021-07-16 | 重庆大学 | MoS2PEO humidity sensor, double-device humidity sensing device and humidity detection method |
| CN114813855A (en) * | 2022-03-31 | 2022-07-29 | 郑州大学 | Carbon dot-based humidity sensor and preparation method thereof |
| CN116443856A (en) * | 2023-03-28 | 2023-07-18 | 上海大学 | Carbon quantum dot/MoS 2 Nanosheet composite material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107064242A (en) * | 2017-04-11 | 2017-08-18 | 西南交通大学 | Molybdenum disulfide dopen Nano silver particles are combined humidity sensor and preparation method thereof |
-
2017
- 2017-12-14 CN CN201711339515.4A patent/CN108169284B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107064242A (en) * | 2017-04-11 | 2017-08-18 | 西南交通大学 | Molybdenum disulfide dopen Nano silver particles are combined humidity sensor and preparation method thereof |
Non-Patent Citations (4)
| Title |
|---|
| JING WANG 等: "One-pot synthesis of multifunctional magnetic ferrite-MoS2-carbon dots nanohybrid adsorbent for efficient Pb(II) removal", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
| JINZHU WU 等: "Carbon dot-assisted hydrothermal synthesis of flower-like MoS2 nanospheres constructed by few-layered multiphase MoS2 nanosheets for supercapacitors", 《RSC ADVANCES》 * |
| MINGHAN XU 等: "One-pot liquid-phase exfoliation from graphite to graphene with carbon quantum dots", 《NANOSCALE》 * |
| XING ZHANG 等: "Highly sensitive humidity sensing properties of carbon quantum dots films", 《MATERIALS RESEARCH BULLETIN》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108786857A (en) * | 2018-07-06 | 2018-11-13 | 中北大学 | A kind of carbon dots/two dimension MoS2Composite photo-catalyst and preparation method thereof |
| CN108786857B (en) * | 2018-07-06 | 2021-04-30 | 中北大学 | Carbon dot/two-dimensional MoS2Composite photocatalyst and preparation method thereof |
| CN110208337A (en) * | 2019-06-28 | 2019-09-06 | 西南交通大学 | Compound humidity sensor of molybdenum disulfide/Nano diamond and preparation method thereof |
| CN110208337B (en) * | 2019-06-28 | 2022-02-08 | 西南交通大学 | Molybdenum disulfide/nano diamond composite humidity sensor and preparation method thereof |
| CN110228821A (en) * | 2019-07-12 | 2019-09-13 | 安徽大学 | A kind of preparation method that carbon dots doping induces 1T phase molybdenum disulfide and the application in energy storage material |
| CN113029239A (en) * | 2021-03-11 | 2021-06-25 | 昆山联鲸仪智能科技有限公司 | Multifunctional sensor and preparation method thereof |
| CN113125520A (en) * | 2021-04-21 | 2021-07-16 | 重庆大学 | MoS2PEO humidity sensor, double-device humidity sensing device and humidity detection method |
| CN114813855A (en) * | 2022-03-31 | 2022-07-29 | 郑州大学 | Carbon dot-based humidity sensor and preparation method thereof |
| CN116443856A (en) * | 2023-03-28 | 2023-07-18 | 上海大学 | Carbon quantum dot/MoS 2 Nanosheet composite material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108169284B (en) | 2021-01-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108169284B (en) | Humidity sensor based on carbon dot doped molybdenum disulfide sheet and preparation method thereof | |
| Chen et al. | Effects of morphologies on acetone-sensing properties of tungsten trioxide nanocrystals | |
| Ma et al. | Ultrahigh sensitivity and selectivity chlorine gas sensing of In2O3 hollow microtubules by bio-template method with degreasing cotton | |
| Liu et al. | Facile synthesis and NO2 gas sensing of tungsten oxide nanorods assembled microspheres | |
| Hou et al. | Low resistive aluminum doped nanocrystalline zinc oxide for reducing gas sensor application via sol–gel process | |
| Abu-Hani et al. | Design, fabrication, and characterization of low-power gas sensors based on organic-inorganic nano-composite | |
| Fu | Sensing behavior of CdS nanoparticles to SO2, H2S and NH3 at room temperature | |
| CN103852494A (en) | Method for preparing nitrogen dioxide gas sensor element with ultra-fast response characteristics | |
| Hsu et al. | Rapid synthesis of ZnO dandelion-like nanostructures and their applications in humidity sensing and photocatalysis | |
| Liu et al. | Au-decorated In2O3 nanospheres/exfoliated Ti3C2Tx MXene nanosheets for highly sensitive formaldehyde gas sensing at room temperature | |
| Prakash et al. | Sensing properties of ZnO nanoparticles synthesized by using albumen as a biotemplate for acetic acid monitoring in aqueous mixture | |
| Khatibani | Investigation of gas sensing property of zinc oxide thin films deposited by Sol-Gel method: effects of molarity and annealing temperature | |
| Munusami et al. | Development of high sensitivity LPG and NO2 gas sensor based ZnGa2O4/graphene nanoplates hybrid structure-A novel approach | |
| CN102012386A (en) | Preparation method of nitric oxide gas sensor element based on pseudodirected tungsten trioxide nano tape | |
| Chaudhary et al. | Preparation of carbon quantum dots using bike pollutant soot: Evaluation of structural, optical and moisture sensing properties | |
| Xu et al. | Design of MoS2/ZnO bridge-like hetero-nanostructures to boost triethylamine (TEA) sensing | |
| Pawar et al. | Facile green synthesis of In 2 O 3 bricks and its NO 2 gas sensing properties | |
| Han et al. | Cu2O template-assisted synthesis of porous In2O3 hollow spheres with fast response towards acetone | |
| Zhang et al. | Response improvement for In2O3–TiO2 thick film gas sensors | |
| Patil et al. | NH 3 gas sensing performance of ternary TiO 2/SnO 2/WO 3 hybrid nanostructures prepared by ultrasonic-assisted sol–gel method | |
| Benzitouni et al. | High sensitivity of porous Cu-doped SnO 2 thin films to methanol | |
| Tang et al. | In 2 O 3 nanostructures: synthesis and chlorobenzene sensing properties | |
| Foo et al. | Au decorated ZnO thin film: application to DNA sensing | |
| Li et al. | Improvement of Voltammetric Detection of Sulfanilamide with a Nanodiamond-Modified Glassy Carbon Electrode | |
| Lei et al. | Three-dimensional hierarchical CuO gas sensor modified by Au nanoparticles |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |