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
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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 present invention relates to gas sensing techniques field more particularly to a kind of molybdenum disulfide thin slices based on carbon dots doping vario-property
Humidity sensor and preparation method thereof.
Background technology
Humidity is the important parameter of environmental assessment, because it suffers from inseparable connection with many things in environment
System.In addition to this, humidity suffers from very important influence to industrial production and technology development.The measure of humidity and continuous monitoring
To many fields such as semiconductor manufacturing, packaging industry, monitoring soil moisture, pharmacy and food processing, civil engineering, electronics add
Work, household electrical appliance and air-conditioning system are all particularly significant.According to a nearest investigation display, to the year two thousand twenty humidity sensor market part
Volume occupancy volume is estimated to be up to 2,300,000,000 dollars.It can be seen that developing, response is fast, and high sensitivity, test scope is wide, cost
Low humidity sensor is the active demand of current social development.
Humidity sensor material in currently commercially widest humidity sensor is porous ceramics and polymer film.
Polymer sensing material exists and cannot be run under high humidity level, display lag, low-response and is easy to run off etc. being difficult to for a long time
The shortcomings that overcoming.Commercial humidity sensor can also use metal oxide as inductive layer, and shortcoming is to need periodically to carry out heat clearly
It washes to restore its humidity sensor characteristic.In addition, due to hydroxyl ion in gradual chemisorbed on the surface of inductive layer, so as to lead
Gradually changing for its resistance is caused, so as to lower the humidity sensor performance of inductive layer.Now, it is high to be devoted to exploitation for many seminar
The humidity sensor nano material of performance, such as nano-silicon, nano ceramics, semiconductor nanoparticle and metal oxide nano-wire etc.,
Practical application is there are of high cost, the deficiencies of being not easy to realize extensive use.
In the prior art, the two-dimensional metallic sulfide molybdenum disulfide of class graphene-structured is due to its larger specific surface area,
The advantages such as high electron mobility and conductivity, low background noise also possess very big potentiality in gas sensing field.But
It is that the substrate surface of two-dimentional molybdenum disulfide is catalytically inactive, active site position is only in the position at layer edge, and original two sulphur
Change molybdenum surface also without active function groups, it is extremely limited to the uptake of hydrone that these have resulted in molybdenum disulfide, actually makes
Used time causes the electron transmission between molybdenum disulfide and hydrone that can not continuously continue to carry out, and eventually leads to based on molybdenum disulfide
Humidity sensor shows the sensing defect that susceptibility is low, and the response time is grown.
Therefore, those skilled in the art is dedicated to developing a kind of humidity sensor based on carbon dots doping molybdenum disulfide thin slice
Device and preparation method thereof.
Invention content
In view of the drawbacks described above of the prior art, the technical problems to be solved by the invention are existing molybdenum disulfide degree sensings
Device is low to humidity response sensitivity, and the response time is long.
To achieve the above object, the present invention provides a kind of compounds based on carbon dots doping molybdenum disulfide thin slice；
Wherein, the compound of the carbon dots doping molybdenum disulfide thin slice is two-dimensional nano flake.
The present invention also provides a kind of humidity sensors based on carbon dots doping molybdenum disulfide thin slice, and it includes carbon dots doping
The compound of molybdenum disulfide thin slice is as humidity sensor layer.
The present invention also provides a kind of preparation method of the compound based on carbon dots doping molybdenum disulfide thin slice, including following
Step：
Step 1, carbon source is added to the water and prepares carbon dots aqueous solution；
Step 2, molybdenum source reagent and sulphur source reagent are added in the carbon dots aqueous solution that step 1 obtains, using a step hydro-thermal
Prepared by method, post processing obtains the compound of carbon dots doping molybdenum disulfide thin slice.
The present invention also provides a kind of preparation method of the humidity sensor based on carbon dots doping molybdenum disulfide thin slice, packets
Include the preparation method step and following steps of the above-mentioned compound based on carbon dots doping molybdenum disulfide thin slice：
Step 3, the compound of carbon dots doping molybdenum disulfide that step 2 obtains with alcohol reagent is mixed, is added drop-wise to interdigital electricity
On extremely, drying obtains the humidity sensor of carbon dots doping molybdenum disulfide thin slice.
Further, in the step 1, the method for preparing carbon dots aqueous solution is selected from microwave method, hydro-thermal method, high-temperature melting method
In one kind；
Further, in the step 1, carbon source is selected from Pidolidone, cysteine, lysine, tryptophan, in citrulling
It is one or more；
Further, in the step 1, the w/v (mg/ml) of carbon source and water is 10:1~20:1；
Further, in the step 2, molybdenum source reagent is a kind of or more in two molybdic acid hydrate sodium, Ammonium Molybdate Tetrahydrate
Kind combination；
Further, in the step 2, the one or more combinations in thiocarbamide, thioacetamide of sulphur source reagent；
Further, in the step 2, the w/v (mg/ml) of molybdenum source reagent and carbon dots aqueous solution is 20:
1~40:1；
Further, in the step 2, the w/v (mg/ml) of sulphur source reagent and carbon dots aqueous solution is 10:
1~20:1；It is preferred that 13:1；
Further, in the step 2, the reaction temperature of the one step hydro thermal method is 160~240 DEG C, and the reaction time is
12~36h；
Further, in the step 2, post processing includes washing, centrifugation；
Further, the solvent of the washing is a kind of in water, ethyl alcohol or the mixed solvent of water and ethanol composition；It is described
Centrifugal speed is 5000~10000rpm, and centrifugation time is 5~30min；
Further, in the step 3, alcohol reagent is selected from one or more of methanol, ethyl alcohol, propyl alcohol, butanol；
Further, in the step 3, the dropwise addition volume of the compound mixed alkoxide solution of carbon dots doping molybdenum disulfide is 1
~5 μ L；
Further, in the step 3, drying temperature is 50~100 DEG C, and drying time is 0.5~3h.
In the better embodiment of the present invention, in the step 1, the method for preparing carbon dots aqueous solution is hydro-thermal method；Its
In, the reaction temperature of the hydro-thermal method is 200 DEG C, reaction time 12h；
In another better embodiment of the present invention, in the step 1, the method for preparing carbon dots aqueous solution is high temperature melting
Melt method；Wherein, the reaction temperature of high-temperature melting method is 250 DEG C；
In another better embodiment of the present invention, in the step 1, the method for preparing carbon dots aqueous solution is microwave
Method；Wherein, microwave reaction temperature is 200 DEG C, and the microwave reaction time is 30min；
In another better embodiment of the present invention, in the step 1, the w/v (milligram/milli of carbon source and water
Rise) it is 10:1；
In another better embodiment of the present invention, in the step 1, the w/v (milligram/milli of carbon source and water
Rise) it is 20:1；
In another better embodiment of the present invention, in the step 1, the w/v (milligram/milli of carbon source and water
Rise) it is 13:1；
In another better embodiment of the present invention, in the step 2, the weighing body of molybdenum source reagent and carbon dots aqueous solution
Product is 20 than (mg/ml):1；
In another better embodiment of the present invention, in the step 2, the weighing body of molybdenum source reagent and carbon dots aqueous solution
Product is 30 than (mg/ml):1；
In another better embodiment of the present invention, in the step 2, the weighing body of molybdenum source reagent and carbon dots aqueous solution
Product is 40 than (mg/ml):1；
In another better embodiment of the present invention, in the step 2, the weighing body of sulphur source reagent and carbon dots aqueous solution
Product is 13 than (mg/ml):1；
In another better embodiment of the present invention, in the step 2, the reaction temperature of the one step hydro thermal method is
200 DEG C, the reaction time is for 24 hours；
In another better embodiment of the present invention, in the step 3, alcohol reagent is ethyl alcohol；
In another better embodiment of the present invention, in the step 3, drying temperature is 60 DEG C, and drying time is
0.5h。
The present invention also provides described in any of the above-described of the present invention based on carbon dots doping molybdenum disulfide thin slice compound, with
And any one preparation method be prepared based on carbon dots doping molybdenum disulfide foil laminates prepare for humidity sensor supervise
Purposes in survey.
The present invention also provides the humidity sensors based on carbon dots doping molybdenum disulfide thin slice described in any of the above-described of the present invention
The humidity sensor based on carbon dots doping molybdenum disulfide thin slice that device and any one preparation method are prepared is used in preparation
Purposes in humidity sensor monitoring.
Using above scheme, compound, humidity sensor disclosed by the invention based on carbon dots doping molybdenum disulfide thin slice
And preparation method, it has the following advantages：
The present invention based on carbon dots doping molybdenum disulfide thin slice compound preparation process it is simple, raw material sources extensively and
It is cheap, easily realize industrialized production and application；
The present invention's adulterates the compound of molybdenum disulfide thin slice and its humidity sensor of preparation in room temperature item based on carbon dots
Response sensitivity height is shown under part to the humidity in environment, fast response time shows cutting edge aligned sound in certain measurement range
Should, there is excellent humidity response performance；
The compound based on carbon dots doping molybdenum disulfide thin slice of the present invention, compared with existing humidity sensor nano material
Compared with, it is low with manufacturing cost, it is environmentally protective, use cost can be reduced to greatest extent in practical applications, it can extensive use
Field is monitored in different moisture levels, there is great application prospect.
The technique effect of the design of the present invention, specific technical solution and generation is made into one below with reference to preferred embodiment
Step explanation, to be fully understood from the purpose of the present invention, feature and effect.
Description of the drawings
Fig. 1 is the scanning electron microscope diagram of the compound based on carbon dots doping molybdenum disulfide thin slice of embodiment 1；
Fig. 2 is the humidity sensor based on carbon dots doping molybdenum disulfide thin slice of embodiment 1 under 75% relative humidity
Humidity responds Repeatability figure；
Fig. 3 is humidity sensor of the embodiment 1 based on carbon dots doping molybdenum disulfide thin slice to carrying out humidity under different humidity
Detect response performance figure；
Fig. 4 is humidity sensor of the embodiment 1 based on carbon dots doping molybdenum disulfide thin slice to carrying out humidity under different humidity
Detection response Linear Fit Chart.
Specific embodiment
Multiple preferred embodiments of the present invention introduced below make its technology contents more clear and are easy to understand.The present invention
Can be emerged from by many various forms of embodiments, these embodiments be exemplary description, protection model of the invention
Enclose the embodiment for being not limited only to mention in text.
If there is test method without specific conditions, usually according to normal condition, such as instructions book or handbook
Implemented.
Embodiment 1, based on carbon dots doping molybdenum disulfide thin slice compound and humidity sensor preparation
Step 1, the Pidolidone of 300mg is added in 30mL water, is transferred in reaction kettle after being uniformly dispersed, 200 DEG C
12h is heated, cooling obtains carbon dots aqueous solution；
Step 2, by the sodium molybdate of 900mg, the thiocarbamide of 390mg is added to the 30mL carbon dots aqueous solutions that above-mentioned steps 1 obtain
In, dispersion is transferred to after obtaining uniform solution in reaction kettle.200 DEG C of heating for 24 hours, are obtained based on carbon dots doping molybdenum disulfide
Composite solids crude product；
For solid crude product respectively with alternately washing 3 times of deionized water and ethyl alcohol, centrifugal speed is to centrifuge 10min under 7000rpm
Obtain the compound based on carbon dots doping molybdenum disulfide thin slice；
Step 3, the compound based on carbon dots doping molybdenum disulfide thin slice that step 2 obtains is dissolved in absolute ethyl alcohol, liquid relief
Rifle measures 2 μ L and is added drop-wise in interdigital electrode, treats that ethyl alcohol volatilization is complete, and electrode is put into 60 DEG C of drying 0.5h in baking oven is based on
Carbon dots adulterate the humidity sensor of molybdenum disulfide thin slice.
The compound based on carbon dots doping molybdenum disulfide thin slice that step 2 obtains is subjected to electron microscope scanning, such as Fig. 1
Shown, the compound pattern based on carbon dots doping molybdenum disulfide thin slice of the present embodiment is uniform, is made of two-dimensional nano thin slice.
Embodiment 2, based on carbon dots doping molybdenum disulfide thin slice compound and humidity sensor preparation
Step 1, the Pidolidone of 1200mg is added in round-bottomed flask, is heated to 250 DEG C, until Pidolidone melts
Into yellowish-brown liquid, 90mL deionized waters are added in, bulky grain is centrifuged off after dissolving, obtains carbon dots aqueous solution；
Step 2, by the sodium molybdate of 600mg, the thiocarbamide of 390mg is added to the 30mL carbon dots aqueous solutions that above-mentioned steps 1 obtain
In, dispersion is transferred to after obtaining uniform solution in reaction kettle.160 DEG C of heating 36h are obtained based on carbon dots doping molybdenum disulfide
Composite solids crude product；
For solid crude product respectively with alternately washing 3 times of deionized water and ethyl alcohol, centrifugal speed is to centrifuge 30min under 5000rpm
Obtain the compound based on carbon dots doping molybdenum disulfide thin slice.
Step 3, the compound based on carbon dots doping molybdenum disulfide thin slice that step 2 obtains is dissolved in absolute ethyl alcohol, liquid relief
Rifle measures 2 μ L and is added drop-wise in interdigital electrode, treats that ethyl alcohol volatilization is complete, and electrode is put into 80 DEG C of drying 3h in baking oven obtains based on carbon
The humidity sensor of point doping molybdenum disulfide thin slice.
Embodiment 3, based on carbon dots doping molybdenum disulfide thin slice compound and humidity sensor preparation
Step 1, the L-cysteine of 300mg is added in 15mL water, is transferred to after being uniformly dispersed in microwave reaction bottle,
200 DEG C of microwave reaction 30min, obtain carbon dots aqueous solution；
Step 2, by the sodium molybdate of 1200mg, the thiocarbamide of 390mg is added to the 30mL carbon dots aqueous solutions that above-mentioned steps 1 obtain
In, dispersion is transferred to after obtaining uniform solution in reaction kettle.240 DEG C of heating 12h are obtained based on carbon dots doping molybdenum disulfide
Composite solids crude product；
For solid crude product respectively with alternately washing 3 times of deionized water and ethyl alcohol, centrifugal speed is that centrifugation 8min is obtained under 8000rpm
To the compound based on carbon dots doping molybdenum disulfide thin slice.
Step 3, the compound based on carbon dots doping molybdenum disulfide thin slice that step 2 obtains is dissolved in absolute ethyl alcohol, liquid relief
Rifle measures 2 μ L and is added drop-wise in interdigital electrode, treats that ethyl alcohol volatilization is complete, and electrode is put into 100 DEG C of drying 0.5h in baking oven obtains base
In the humidity sensor of carbon dots doping molybdenum disulfide thin slice.
Test example 4, humidity response detection
(1) humidity sensor of the embodiment 1 based on carbon dots doping molybdenum disulfide thin slice carries out wet under 75% relative humidity
Degree response repeats to detect；
The results are shown in Figure 2, and the humidity sensor based on carbon dots doping molybdenum disulfide thin slice of the embodiment of the present invention 1 exists
Under 75% relative humidity, the detection response curve being repeated 4 times within 2000 second time is basically identical, shows quick response
With good repeatability, show the embodiment of the present invention 1 based on carbon dots doping molybdenum disulfide thin slice humidity sensor response and
Repeatability is excellent.
(2) humidity sensor of the embodiment 1 based on carbon dots doping molybdenum disulfide thin slice carries out humidity sound under different humidity
It should detect；
The results are shown in Figure 3, and the humidity sensor based on carbon dots doping molybdenum disulfide thin slice of the embodiment of the present invention 1 exists
Under 15%~80% relative humidity, stronger response signal is shown, show the embodiment of the present invention 1 adulterates two sulphur based on carbon dots
The humidity sensor for changing molybdenum thin slice has wider response range, can be widely applied to the detection environment of various different humidities.
To humidity sensor of the embodiment 1 based on carbon dots doping molybdenum disulfide thin slice to carrying out humidity response under different humidity
The response of detection carries out linear fit, and the results are shown in Figure 4, the embodiment of the present invention 1 it is thin based on carbon dots doping molybdenum disulfide
The humidity sensor of piece shows linear response under 15%~80% relative humidity；Show the embodiment of the present invention 1 based on carbon
The humidity sensor of point doping molybdenum disulfide thin slice has excellent Humidity Detection performance.
In conclusion the humidity sensor of the humidity sensor based on carbon dots doping molybdenum disulfide thin slice of the embodiment of the present invention
It is excellent to respond Repeatability, there is wider response range and shows linear response, show the embodiment of the present invention based on carbon
The humidity sensor Humidity Detection various aspects of performance of point doping molybdenum disulfide thin slice is excellent.
Other embodiment technical solution of the present invention also has advantageous effect similar to above.
The preferred embodiment of the present invention described in detail above.It should be appreciated that the ordinary skill of this field is without wound
The property made labour, which according to the present invention can conceive, makes many modifications and variations.Therefore, all technician in the art
Pass through logic analysis, reasoning or the available technology of limited experiment on the basis of existing technology under this invention's idea
Scheme, all should be in the protection domain being defined in the patent claims.
Claims (10)
1. a kind of compound based on carbon dots doping molybdenum disulfide thin slice, which is characterized in that the carbon dots doping molybdenum disulfide is thin
The compound of piece is two-dimensional nano flake.
2. a kind of humidity sensor based on carbon dots doping molybdenum disulfide thin slice, which is characterized in that the humidity sensor includes
Compound based on carbon dots doping molybdenum disulfide thin slice described in claim 1 is as humidity sensor layer.
3. a kind of preparation method of the compound based on carbon dots doping molybdenum disulfide thin slice, which is characterized in that include the following steps：
Step 1, carbon source is added to the water and prepares carbon dots aqueous solution；
Step 2, molybdenum source reagent and sulphur source reagent are added in the carbon dots aqueous solution that step 1 obtains, using one step hydro thermal method system
Standby, post processing obtains the compound of carbon dots doping molybdenum disulfide thin slice.
4. a kind of preparation method of the humidity sensor based on carbon dots doping molybdenum disulfide thin slice, which is characterized in that including following
Step：
Step 1, carbon source is added to the water and prepares carbon dots aqueous solution；
Step 2, molybdenum source reagent and sulphur source reagent are added in the carbon dots aqueous solution that step 1 obtains, using one step hydro thermal method system
Standby, post processing obtains the compound of carbon dots doping molybdenum disulfide thin slice；
Step 3, the compound of carbon dots doping molybdenum disulfide that step 2 obtains with alcohol reagent is mixed, is added drop-wise in interdigital electrode,
Drying obtains the humidity sensor of carbon dots doping molybdenum disulfide thin slice.
5. the preparation method as described in claim 3 or 4, which is characterized in that
In the step 1, the one kind of the method for carbon dots aqueous solution in microwave method, hydro-thermal method, high-temperature melting method is prepared；
In the step 1, carbon source is selected from Pidolidone, cysteine, lysine, and tryptophan is one or more in citrulling；
In the step 1, the w/v of carbon source and water is 10:1~30:1.
6. the preparation method as described in claim 3 or 4, which is characterized in that
In the step 2, the one or more combinations in two molybdic acid hydrate sodium, Ammonium Molybdate Tetrahydrate of molybdenum source reagent；
In the step 2, the one or more combinations in thiocarbamide, thioacetamide of sulphur source reagent；
In the step 2, the w/v of molybdenum source reagent and carbon dots aqueous solution is 20:1~40:1；
In the step 2, the w/v of sulphur source reagent and carbon dots aqueous solution is 10:1~20:1；
In the step 2, the reaction temperature of the one step hydro thermal method is 160~240 DEG C, and the reaction time is 12~36h；
In the step 2, post processing includes washing, centrifugation；The solvent of the washing a kind of or water and ethyl alcohol in water, ethyl alcohol
The mixed solvent of combination；The centrifugal speed is 5000~10000rpm, and centrifugation time is 5~30min.
7. the preparation method as described in claim 3 or 4, which is characterized in that
In the step 3, alcohol reagent is selected from one or more of methanol, ethyl alcohol, propyl alcohol, butanol；
In the step 3, the compound of carbon dots doping molybdenum disulfide and the dropwise addition volume of alcohol mixture are 1~5 μ L；
In the step 3, drying temperature is 50~100 DEG C, and drying time is 0.5~3h.
8. the compound based on carbon dots doping molybdenum disulfide thin slice that preparation method described in a kind of claim 3 obtains, feature
It is, the compound of the carbon dots doping molybdenum disulfide thin slice is two-dimensional nano flake.
9. the humidity sensor based on carbon dots doping molybdenum disulfide thin slice that preparation method described in a kind of claim 4 obtains,
It is characterized in that, includes the following steps：
Step 1, carbon source is added to the water and prepares carbon dots aqueous solution；
Step 2, molybdenum source reagent and sulphur source reagent are added in the carbon dots aqueous solution that step 1 obtains, using one step hydro thermal method system
Standby, post processing obtains the compound of carbon dots doping molybdenum disulfide thin slice；
Step 3, the compound of carbon dots doping molybdenum disulfide that step 2 obtains with alcohol reagent is mixed, is added drop-wise in interdigital electrode,
Drying obtains the humidity sensor of carbon dots doping molybdenum disulfide thin slice；
Wherein,
In the step 1, the one kind of the method for carbon dots aqueous solution in microwave method, hydro-thermal method, high-temperature melting method is prepared；
In the step 1, carbon dots raw material is selected from Pidolidone, cysteine, lysine, tryptophan, one kind in citrulling or
It is a variety of；
In the step 1, the w/v of carbon source and water is 10:1~30:1；
In the step 2, the one or more combinations in two molybdic acid hydrate sodium, Ammonium Molybdate Tetrahydrate of molybdenum source reagent；
In the step 2, the one or more combinations in thiocarbamide, thioacetamide of sulphur source reagent；
In the step 2, the w/v of molybdenum source reagent and carbon dots aqueous solution is 20:1~40:1；
In the step 2, the w/v of sulphur source reagent and carbon dots aqueous solution is 10:1~20:1；
In the step 2, the reaction temperature of the one step hydro thermal method is 160~240 DEG C, and the reaction time is 12~36h；
In the step 2, post processing includes washing, centrifugation；The solvent of the washing a kind of or water and ethyl alcohol in water, ethyl alcohol
The mixed solvent of combination；The centrifugal speed is 5000~10000rpm, and centrifugation time is 5~30min；
In the step 3, alcohol reagent is selected from one or more of methanol, ethyl alcohol, propyl alcohol, butanol；
In the step 3, the compound of carbon dots doping molybdenum disulfide and the dropwise addition volume of alcohol mixture are 1~5 μ L；
In the step 3, drying temperature is 50~100 DEG C, and drying time is 0.5~3h.
10. the compound of molybdenum disulfide thin slice or claim 2,9 are adulterated based on carbon dots described in claim 1,8 any one
Humidity sensor based on carbon dots doping molybdenum disulfide thin slice described in one is prepared for the purposes in humidity sensor monitoring.
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| 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 |
| 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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