CN107064242A - Molybdenum disulfide dopen Nano silver particles are combined humidity sensor and preparation method thereof - Google Patents
Molybdenum disulfide dopen Nano silver particles are combined humidity sensor and preparation method thereof Download PDFInfo
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- CN107064242A CN107064242A CN201710233104.0A CN201710233104A CN107064242A CN 107064242 A CN107064242 A CN 107064242A CN 201710233104 A CN201710233104 A CN 201710233104A CN 107064242 A CN107064242 A CN 107064242A
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- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/22—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance
- G01N27/223—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance for determining moisture content, e.g. humidity
Abstract
The present invention provides a kind of molybdenum disulfide dopen Nano silver particles and is combined humidity sensor and preparation method thereof, including step：Nano silver particles aqueous dispersions are formed, nano silver particles aqueous dispersions are mixed in molybdenum disulfide aqueous dispersions, ultrasonic disperse obtains molybdenum disulfide doping nano-Ag particle composite material dispersion liquid；In silicon substrate surface formation layer of silicon dioxide layer; so in silica layer surface formation first electrode and second electrode; obtain electrode base sheet; the molybdenum disulfide doping nano-Ag particle composite material dispersion liquid obtained; it is attached to electrode base sheet surface; it is placed into stand in protective gas and processing is dried, so as to obtains being attached with the electrode base sheet of molybdenum disulfide doping nano-Ag particle composite material film；The humidity sensor of the present invention has higher response sensitivity and faster response speed.
Description
Technical field
Field is manufactured the present invention relates to sensor, is related specifically to a kind of with hypersensitivity, the spy of fast-response speed
The molybdenum disulfide dopen Nano silver particles of point are combined humidity sensor and preparation method thereof.
Background technology
Humidity sensor is widely used in various fields, but still there are some problems, such as relatively low response sensitivity,
Longer response time and recovery time etc..
2013, Yinghua Tan were in article The combinations of hollow MoS2 micro@
nanospheres:one-step synthesis,excellent photocatalytic and humidity sensing
A kind of Relative Humidity Sensor based on pure molybdenum disulfide is proposed in properties, the sensor electrode unit is
Plane double pectination interdigital structures arranged side by side, are coated in electrode zone, this humidity sensor uses two sulphur by molybdenum disulfide dispersant liquid drop
Change molybdenum as sensitive material, have benefited from the larger specific surface area of molybdenum disulfide, the sensor is compared in the past based on traditional material
Such as the humidity sensor of polyimides, lithium chloride and oxide ceramic material etc. has higher humidity response sensitivity,
But also only have tens pico farads per relative humidity response change, and sensor response time more than 100 seconds, be limited to
Molybdenum disulfide material self character, the sensitivity of this humidity sensor and response speed are difficult to further raising.
The content of the invention
The shortcoming of prior art in view of the above, it is an object of the invention to provide one kind have higher sensitivity and compared with
The molybdenum disulfide dopen Nano silver particles of fast-response speed are combined humidity sensor and preparation method thereof.
For achieving the above object, technical solution of the present invention is as follows：
A kind of molybdenum disulfide dopen Nano silver particles are combined the preparation method of humidity sensor, comprise the following steps：
(1) it is 0.1~4.0 milligram/milli to be less than or equal to 100 nanometers of nano silver particles to mix formation concentration in water by particle diameter
The nano silver particles aqueous dispersions risen, are 0.1~4.0 mg/ml by the nano silver particles aqueous dispersions incorporation of concentration
In molybdenum disulfide aqueous dispersions, the nano silver particles aqueous dispersions of incorporation and the volume ratio of molybdenum disulfide aqueous dispersions are less than or equal to
1:5 and more than or equal to 1:20, ultrasonic disperse 2~24 hours obtains molybdenum disulfide doping nano-Ag particle composite material dispersion liquid；
(2) silicon chip is cleaned up, in silicon substrate surface thermal oxidation method formation layer of silicon dioxide layer, then with true
Empty coating method obtains electrode base sheet in silica layer surface formation first electrode and second electrode, the first electrode and the
Two electrodes are gold electrode；
(3) the molybdenum disulfide doping nano-Ag particle composite material obtained in the step of taking 1.0~10.0 microlitres (1) disperses
Liquid, the electrode base sheet surface obtained in step (2) is attached to using cladding process, the electrode base sheet then is placed into not higher than 50
DEG C protective gas in stand processing is dried within 1~2 hour so that obtaining surface attachment has one layer of molybdenum disulfide dopen Nano
The electrode base sheet of silver particles composite material film；
(4) there is one layer of molybdenum disulfide dopen Nano silver particles composite wood by the surface attachment obtained in measuring process (3)
Expect the capacitance variations between the first electrode and second electrode of the electrode base sheet of film to measure humidity.
In the step (1), the nano silver particles aqueous dispersions of incorporation and the volume ratio of molybdenum disulfide aqueous dispersions are more than
1：When 5, due to percolation threshold effect, the situation that cliff of displacement formula declines occurs in the basic electric capacity of the sensor of preparation, it is impossible to
Use.When the nano silver particles aqueous dispersions of incorporation and the volume ratio of molybdenum disulfide aqueous dispersions are less than 1：When 20, silver granuel
Sub- ratio is too small, and the sensitivity to sensor improves very limited.
It is preferred that, the Vacuum Coating method in step (2) is evaporation coating method or sputter coating method.
It is preferred that, the cladding process in step (3) is drop-coating, spin-coating method or spraying process one kind therein.
It is preferred that, the protective gas in step (3) is nitrogen.
For achieving the above object, the present invention provides a kind of molybdenum disulfide dopen Nano silver particles and is combined humidity sensor
Device, it uses above-mentioned any one methods described to prepare.
It is preferred that, the compound humidity sensor includes：Silica above the silicon chip of bottom, silicon chip
The curing of between layer, the first electrode of silica layer surface and second electrode, first electrode and second electrode and upper surface
Molybdenum doping nano silver particles composite material film.
It is preferred that, electrode pattern is comb teeth-shaped and to be staggered in electrode base sheet, i.e., adjacent first electrode it
Between be provided with second electrode, first electrode is provided between adjacent second electrode.
Beneficial effects of the present invention are：Humidity sensor proposed by the present invention is multiple using molybdenum disulfide dopen Nano silver particles
Condensation material film is as humidity sensitive medium, and the nano silver particles that particle diameter is less than or equal to 100 nanometers are doped into molybdenum disulfide material
The site of Water Molecular Adsorption is added, facilitates the absorption and the formation of liquid water layer of sensitive media surface and internal water molecule, and
The specific surface area of sensitive thin-film material can be increased, these reasons cause the humidity sensor have higher response sensitivity with
And faster response speed.
Brief description of the drawings
Fig. 1 is that the molybdenum disulfide dopen Nano silver particles of the present invention are combined the sectional view of humidity sensor；
Fig. 2 is that the molybdenum disulfide dopen Nano silver particles of the present invention are combined the electrode structure top view of humidity sensor；
Fig. 3 is that the molybdenum disulfide dopen Nano silver particles of the present invention are combined the top view of humidity sensor；
Fig. 4 is that the molybdenum disulfide dopen Nano silver particles of the present invention are combined the wet sensitive response capacitance data of humidity sensor
Figure；
Fig. 5 is that the molybdenum disulfide dopen Nano silver particles of the present invention are combined the wet sensitive response time data of humidity sensor
Figure.
Wherein, 1 is silicon chip, and 2 be silicon dioxide layer, and 3 be first electrode, and 4 be second electrode, and 5 be that molybdenum disulfide adulterates
Nano silver particles composite material film, 51 be molybdenum disulfide nano sheet, and 52 be nano silver particles.
Embodiment
Illustrate embodiments of the present invention below by way of specific instantiation, those skilled in the art can be by this specification
Disclosed content understands other advantages and effect of the present invention easily.The present invention can also pass through specific realities different in addition
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints with application, without departing from
Various modifications or alterations are carried out under the spirit of the present invention.
Embodiment 1
A kind of molybdenum disulfide dopen Nano silver particles are combined the preparation method of humidity sensor, comprise the following steps：
(1) it is 0.1 mg/ml to be less than or equal to 100 nanometers of nano silver particles to mix formation concentration in water by particle diameter
Nano silver particles aqueous dispersions, by the molybdenum disulfide water that the nano silver particles aqueous dispersions incorporation of concentration is 0.1 mg/ml
In dispersion liquid, the molybdenum disulfide aqueous dispersions of incorporation and the volume ratio of nano silver particles aqueous dispersions are respectively 5:1、10:1、15:
1、20:1,4 samples are obtained, ultrasonic disperse 2 hours obtains molybdenum disulfide doping nano-Ag particle composite material dispersion liquid；
(2) silicon chip is cleaned up, in silicon substrate surface thermal oxidation method formation layer of silicon dioxide layer, then with true
Empty coating method obtains electrode base sheet in silica layer surface formation first electrode and second electrode, the first electrode and the
Two electrodes are gold electrode；
(3) the molybdenum disulfide doping nano-Ag particle composite material dispersion liquid obtained in the step of taking 1.0 microlitres (1), profit
The electrode base sheet surface obtained in step (2) is attached to cladding process, the electrode base sheet is then placed into not higher than 50 DEG C
Stood in protective gas and processing is dried in 1 hour, so that obtaining surface attachment there are one layer of molybdenum disulfide dopen Nano silver particles
The electrode base sheet of composite material film；
(4) there is one layer of molybdenum disulfide dopen Nano silver particles composite wood by the surface attachment obtained in measuring process (3)
Expect the capacitance variations between the first electrode and second electrode of the electrode base sheet of film to measure humidity.
Specifically, the Vacuum Coating method in step (2) is evaporation coating method.
Specifically, the cladding process in step (3) is drop-coating.
Specifically, the protective gas in step (3) is nitrogen.
As shown in Figure 1, Figure 3, the molybdenum disulfide dopen Nano silver particles prepared using the above method are combined humidity and passed
Sensor, including：Silicon chip 1, the silicon dioxide layer 2 of the top of silicon chip 1, the and of first electrode 3 on the surface of silicon dioxide layer 2 of bottom
The molybdenum disulfide doping nano-Ag particle composite material of between second electrode 4, first electrode 3 and second electrode 4 and upper surface is thin
There are molybdenum disulfide nano sheet 51 and nano silver particles 52 in film 5, molybdenum disulfide doping nano-Ag particle composite material film 5.
As shown in Fig. 2 electrode pattern is comb teeth-shaped and is staggered in electrode base sheet, i.e., set between adjacent first electrode
Have and first electrode is provided between second electrode, adjacent second electrode.
Embodiment 2
A kind of molybdenum disulfide dopen Nano silver particles are combined the preparation method of humidity sensor, comprise the following steps：
(1) it is 4.0 mg/mls to be less than or equal to 100 nanometers of nano silver particles to mix formation concentration in water by particle diameter
Nano silver particles aqueous dispersions, by the molybdenum disulfide water that the nano silver particles aqueous dispersions incorporation of concentration is 4.0 mg/mls
In dispersion liquid, the molybdenum disulfide aqueous dispersions of incorporation and the volume ratio of nano silver particles aqueous dispersions are respectively 5:1、10:1、15:
1、20:1,4 samples are obtained, ultrasonic disperse 24 hours obtains molybdenum disulfide doping nano-Ag particle composite material dispersion liquid；
(2) silicon chip is cleaned up, in silicon substrate surface thermal oxidation method formation layer of silicon dioxide layer, then with true
Empty coating method obtains electrode base sheet in silica layer surface formation first electrode and second electrode, the first electrode and the
Two electrodes are gold electrode；
(3) the molybdenum disulfide doping nano-Ag particle composite material dispersion liquid obtained in the step of taking 10.0 microlitres (1), profit
The electrode base sheet surface obtained in step (2) is attached to cladding process, the electrode base sheet is then placed into not higher than 50 DEG C
Stood in protective gas and processing is dried in 2 hours, so that obtaining surface attachment there are one layer of molybdenum disulfide dopen Nano silver particles
The electrode base sheet of composite material film；
(4) there is one layer of molybdenum disulfide dopen Nano silver particles composite wood by the surface attachment obtained in measuring process (3)
Expect the capacitance variations between the first electrode and second electrode of the electrode base sheet of film to measure humidity.
Specifically, the Vacuum Coating method in step (2) is sputter coating method.
Specifically, the cladding process in step (3) is spin-coating method.
Specifically, the protective gas in step (3) is nitrogen.
As shown in Figure 1, Figure 3, the molybdenum disulfide dopen Nano silver particles prepared using the above method are combined humidity and passed
Sensor, including：Silicon chip 1, the silicon dioxide layer 2 of the top of silicon chip 1, the and of first electrode 3 on the surface of silicon dioxide layer 2 of bottom
The molybdenum disulfide doping nano-Ag particle composite material of between second electrode 4, first electrode 3 and second electrode 4 and upper surface is thin
There are molybdenum disulfide nano sheet 51 and nano silver particles 52 in film 5, molybdenum disulfide doping nano-Ag particle composite material film 5.
As shown in Fig. 2 electrode pattern is comb teeth-shaped and is staggered in electrode base sheet, i.e., set between adjacent first electrode
Have and first electrode is provided between second electrode, adjacent second electrode.
Embodiment 3
A kind of molybdenum disulfide dopen Nano silver particles are combined the preparation method of humidity sensor, comprise the following steps：
(1) particle diameter is less than or equal to 100 nanometers of nano silver particles and mixes formation concentration receiving for 2 mg/mls in water
Rice silver particles aqueous dispersions, the nano silver particles aqueous dispersions incorporation of concentration is dissipated for the molybdenum disulfide moisture of 2 mg/mls
In liquid, the molybdenum disulfide aqueous dispersions of incorporation and the volume ratio of nano silver particles aqueous dispersions are respectively 5:1、10:1、15:1、
20:1,4 samples are obtained, ultrasonic disperse 13 hours obtains molybdenum disulfide doping nano-Ag particle composite material dispersion liquid；
(2) silicon chip is cleaned up, in silicon substrate surface thermal oxidation method formation layer of silicon dioxide layer, then with true
Empty coating method obtains electrode base sheet in silica layer surface formation first electrode and second electrode, the first electrode and the
Two electrodes are gold electrode；
(3) the molybdenum disulfide doping nano-Ag particle composite material dispersion liquid obtained in the step of taking 6 microlitres (1), is utilized
Cladding process is attached to the electrode base sheet surface obtained in step (2), and then the electrode base sheet is placed into not higher than 50 DEG C of guarantor
Stood in shield gas and processing is dried in 1.5 hours, so that obtaining surface attachment there are one layer of molybdenum disulfide dopen Nano silver particles
The electrode base sheet of composite material film；
(4) there is one layer of molybdenum disulfide dopen Nano silver particles composite wood by the surface attachment obtained in measuring process (3)
Expect the capacitance variations between the first electrode and second electrode of the electrode base sheet of film to measure humidity.
Specifically, the Vacuum Coating method in step (2) is evaporation coating method.
Specifically, the cladding process in step (3) is spraying process.
Specifically, the protective gas in step (3) is nitrogen.
As shown in Figure 1, Figure 3, the molybdenum disulfide dopen Nano silver particles prepared using the above method are combined humidity and passed
Sensor, including：Silicon chip 1, the silicon dioxide layer 2 of the top of silicon chip 1, the and of first electrode 3 on the surface of silicon dioxide layer 2 of bottom
The molybdenum disulfide doping nano-Ag particle composite material of between second electrode 4, first electrode 3 and second electrode 4 and upper surface is thin
There are molybdenum disulfide nano sheet 51 and nano silver particles 52 in film 5, molybdenum disulfide doping nano-Ag particle composite material film 5.
As shown in Fig. 2 electrode pattern is comb teeth-shaped and is staggered in electrode base sheet, i.e., set between adjacent first electrode
Have and first electrode is provided between second electrode, adjacent second electrode.
Performance evaluation
Fig. 4 is that the molybdenum disulfide dopen Nano silver particles of the present invention are combined the wet sensitive response capacitance data of humidity sensor
Figure；As shown in figure 4, the molybdenum disulfide dopen Nano silver particles compound sensor prepared, its electric capacity wet sensitive is responded with curing
The volume ratio increase of molybdenum dispersion liquid and nano silver particles dispersion liquid and increase, and compared to being coated with the identical of same volume
Sensor prepared by the pure molybdenum disulfide dispersion liquid of concentration, its wet sensitive response capacitance improves more than 22 times.Wherein, step
(1) in different samples, the nano silver particles aqueous dispersions of incorporation and the volume ratio of molybdenum disulfide aqueous dispersions are 1:Performance when 5
Most preferably.In the step (1), the nano silver particles aqueous dispersions of incorporation and the volume ratio of molybdenum disulfide aqueous dispersions are more than 1：5
When, due to percolation threshold effect, the situation that cliff of displacement formula declines occurs in the basic electric capacity of the sensor of preparation, it is impossible to make
With.When the nano silver particles aqueous dispersions of incorporation and the volume ratio of molybdenum disulfide aqueous dispersions are less than 1：When 20, silver particles
Ratio is too small, and the sensitivity to sensor improves very limited.
Fig. 5 is that the molybdenum disulfide dopen Nano silver particles of the present invention are combined the wet sensitive response time data of humidity sensor
Figure.Ordinate represents electric capacity, and abscissa represents the response time, and percentage therein represents relative humidity.As shown in figure 5, utilizing
A kind of molybdenum disulfide dopen Nano silver particles compound sensor prepared by the above method, its response time is less than or equal to 2 seconds, compares
In above-mentioned document The combinations of hollow MoS2 micro@nanospheres:one-step
One mentioned in synthesis, excellent photocatalytic and humidity sensing properties
The Relative Humidity Sensor based on pure molybdenum disulfide is planted, response speed has increased significantly.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause
This, all those of ordinary skill in the art without departing from disclosed spirit with being completed under technological thought
All equivalent modifications or change, should by the present invention claim be covered.
Claims (7)
1. a kind of molybdenum disulfide dopen Nano silver particles are combined the preparation method of humidity sensor, it is characterised in that including following step
Suddenly：
(1) it is 0.1~4.0 mg/ml to be less than or equal to 100 nanometers of nano silver particles to mix formation concentration in water by particle diameter
Nano silver particles aqueous dispersions, by two sulphur that the nano silver particles aqueous dispersions incorporation of concentration is 0.1~4.0 mg/ml
Change in molybdenum aqueous dispersions, the nano silver particles aqueous dispersions of incorporation and the volume ratio of molybdenum disulfide aqueous dispersions are less than or equal to 1:5
And more than or equal to 1:20, ultrasonic disperse 2~24 hours obtains molybdenum disulfide doping nano-Ag particle composite material dispersion liquid；
(2) silicon chip is cleaned up, in silicon substrate surface thermal oxidation method formation layer of silicon dioxide layer, then uses Vacuum Deposition
Embrane method obtains electrode base sheet, the first electrode and the second electricity in silica layer surface formation first electrode and second electrode
Extremely gold electrode；
(3) the molybdenum disulfide doping nano-Ag particle composite material dispersion liquid obtained in the step of taking 1.0~10.0 microlitres (1),
The electrode base sheet surface obtained in step (2) is attached to using cladding process, the electrode base sheet is then placed into not higher than 50 DEG C
Protective gas in stand processing is dried within 1~2 hour so that obtaining surface attachment has one layer of molybdenum disulfide doping nano-Ag
The electrode base sheet of particle composite material film；
(4) there is one layer of molybdenum disulfide doping nano-Ag particle composite material thin by the surface attachment obtained in measuring process (3)
Capacitance variations between the first electrode and second electrode of the electrode base sheet of film measure humidity.
2. molybdenum disulfide dopen Nano silver particles according to claim 1 are combined the preparation method of humidity sensor, it is special
Levy and be：Vacuum Coating method in step (2) is evaporation coating method or sputter coating method.
3. molybdenum disulfide dopen Nano silver particles according to claim 1 are combined the preparation method of humidity sensor, it is special
Levy and be：Cladding process in step (3) is drop-coating, spin-coating method or spraying process one kind therein.
4. molybdenum disulfide dopen Nano silver particles according to claim 1 are combined the preparation method of humidity sensor, it is special
Levy and be：Protective gas in step (3) is nitrogen.
5. a kind of molybdenum disulfide dopen Nano silver particles are combined humidity sensor, it is characterised in that：It uses Claims 1-4
Any one methods described is prepared.
6. molybdenum disulfide dopen Nano silver particles according to claim 5 are combined humidity sensor, it is characterised in that bag
Include：Silicon dioxide layer, the first electrode of silica layer surface and second electrode above the silicon chip of bottom, silicon chip,
The molybdenum disulfide doping nano-Ag particle composite material film of between one electrode and second electrode and upper surface.
7. molybdenum disulfide dopen Nano silver particles according to claim 6 are combined humidity sensor, it is characterised in that：Electrode
Electrode pattern is comb teeth-shaped and is staggered in substrate, i.e., second electrode, adjacent second are provided between adjacent first electrode
First electrode is provided between electrode.
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| CN113418960A (en) * | 2021-05-07 | 2021-09-21 | 电子科技大学 | Flexible humidity sensor based on hydrophilicity-enhanced molybdenum disulfide and preparation method thereof |
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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 |
| CN113125520A (en) * | 2021-04-21 | 2021-07-16 | 重庆大学 | MoS2PEO humidity sensor, double-device humidity sensing device and humidity detection method |
| CN113418960A (en) * | 2021-05-07 | 2021-09-21 | 电子科技大学 | Flexible humidity sensor based on hydrophilicity-enhanced molybdenum disulfide and preparation method thereof |
| CN113735461A (en) * | 2021-09-22 | 2021-12-03 | 西南交通大学 | Quick QCM humidity sensor and application thereof and preparation method of humidity sensor |
| CN113735461B (en) * | 2021-09-22 | 2022-03-25 | 西南交通大学 | Quick QCM humidity sensor and application thereof and preparation method of humidity sensor |
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