CN108169284B - Humidity sensor based on carbon dot doped molybdenum disulfide sheet and preparation method thereof - Google Patents
Humidity sensor based on carbon dot doped molybdenum disulfide sheet and preparation method thereof Download PDFInfo
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- CN108169284B CN108169284B CN201711339515.4A CN201711339515A CN108169284B CN 108169284 B CN108169284 B CN 108169284B CN 201711339515 A CN201711339515 A CN 201711339515A CN 108169284 B CN108169284 B CN 108169284B
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Abstract
The invention discloses a compound based on a carbon dot doped molybdenum disulfide flake, wherein the compound based on the carbon dot doped molybdenum disulfide flake is a two-dimensional nanosheet shape. The invention also provides a preparation method and application of the carbon dot doped molybdenum disulfide flake-based compound. The invention also provides a humidity sensor comprising a carbon dot doped molybdenum disulfide flake-based composite, a preparation method and application thereof. The carbon point doped molybdenum disulfide flake-based compound and the humidity sensor based on the carbon point doped molybdenum disulfide flake compound have the advantages of wide response range, linear response, high response speed, high sensitivity and excellent repeatability.
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 (2)
1. 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 point aqueous solution, wherein the method for preparing the carbon point aqueous solution is one of a microwave method, a hydrothermal method and a high-temperature melting method, the carbon source is one or more of L-glutamic acid, cysteine, lysine, tryptophan and citrulline, and the weight-volume ratio of the carbon source to the water is 10: 1-30: 1;
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;
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.
2. A humidity sensor based on carbon dot doped molybdenum disulfide flake, wherein the humidity sensor comprises a compound based on carbon dot doped molybdenum disulfide flake as a humidity sensing layer, the compound of carbon dot doped molybdenum disulfide flake is a two-dimensional nanosheet, and the humidity sensor is prepared by the preparation method as claimed in claim 1.
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| CN108786857B (en) * | 2018-07-06 | 2021-04-30 | 中北大学 | Carbon dot/two-dimensional MoS2Composite photocatalyst 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 |
| CN113125520B (en) * | 2021-04-21 | 2022-08-12 | 重庆大学 | MoS 2 PEO humidity sensor, double-device humidity sensing device and humidity detection method |
| CN116443856A (en) * | 2023-03-28 | 2023-07-18 | 上海大学 | Carbon quantum dot/MoS 2 Nanosheet composite material and preparation method thereof |
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