CN107064242B - Molybdenum disulfide doped nano silver particle composite humidity sensor and preparation method thereof - Google Patents
Molybdenum disulfide doped nano silver particle composite humidity sensor and preparation method thereof Download PDFInfo
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- CN107064242B CN107064242B CN201710233104.0A CN201710233104A CN107064242B CN 107064242 B CN107064242 B CN 107064242B CN 201710233104 A CN201710233104 A CN 201710233104A CN 107064242 B CN107064242 B CN 107064242B
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Abstract
The invention provides a molybdenum disulfide doped nano silver particle composite humidity sensor and a preparation method thereof, wherein the molybdenum disulfide doped nano silver particle composite humidity sensor comprises the following steps: forming nano silver particle aqueous dispersion, doping the nano silver particle aqueous dispersion into molybdenum disulfide aqueous dispersion, and performing ultrasonic dispersion to obtain molybdenum disulfide-doped nano silver particle composite dispersion; forming a silicon dioxide layer on the surface of a silicon substrate, forming a first electrode and a second electrode on the surface of the silicon dioxide layer to obtain an electrode substrate, taking the obtained molybdenum disulfide doped nano silver particle composite material dispersion liquid, attaching the obtained molybdenum disulfide doped nano silver particle composite material dispersion liquid to the surface of the electrode substrate, placing the electrode substrate in protective gas, standing and drying the electrode substrate to obtain the electrode substrate attached with the molybdenum disulfide doped nano silver particle composite material film; the humidity sensor has high response sensitivity and high response speed.
Description
Technical Field
The invention relates to the field of sensor manufacturing, in particular to a molybdenum disulfide doped nano silver particle composite humidity sensor with the characteristics of ultrahigh sensitivity and high response speed and a preparation method thereof.
Background
Humidity sensors are widely used in various fields, but still have problems such as low response sensitivity, long response time and recovery time, etc.
In 2013, Yinghua Tan in The article The combinations of hole MoS2 micro @ nanospheres: one-step synthesis, isolated photocatalytic and humidity sensing properties, proposes a capacitive relative humidity sensor based on pure molybdenum disulfide, the sensor electrode unit is of a plane parallel double-comb interdigital structure, molybdenum disulfide is dispersed and dripped on an electrode area, the humidity sensor adopts molybdenum disulfide as a sensitive material, benefits from larger specific surface area of the molybdenum disulfide, compared with the traditional humidity sensor based on traditional materials such as polyimide, lithium chloride, oxide ceramic materials and the like, the sensor has higher humidity response sensitivity, however, the response change of each relative humidity is only dozens of picofarads, and the response time of the sensor is more than one hundred seconds, which is limited by the characteristics of the molybdenum disulfide material, and the sensitivity and the response speed of the humidity sensor are difficult to further improve.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention is directed to a molybdenum disulfide-doped nano silver particle composite humidity sensor with high sensitivity and fast response speed and a method for manufacturing the same.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of a molybdenum disulfide doped nano silver particle composite humidity sensor comprises the following steps:
(1) doping nano silver particles with the particle size of less than or equal to 100 nanometers into water to form nano silver particle aqueous dispersion with the concentration of 0.1-4.0 mg/ml, doping the nano silver particle aqueous dispersion into molybdenum disulfide aqueous dispersion with the concentration of 0.1-4.0 mg/ml, wherein the volume ratio of the doped nano silver particle aqueous dispersion to the doped molybdenum disulfide aqueous dispersion is less than or equal to 1:5 and more than or equal to 1:20, and performing ultrasonic dispersion for 2-24 hours to obtain molybdenum disulfide-doped nano silver particle composite dispersion;
(2) cleaning a silicon substrate, forming a silicon dioxide layer on the surface of the silicon substrate by using a thermal oxidation method, and then forming a first electrode and a second electrode on the surface of the silicon dioxide layer by using a vacuum coating method to obtain an electrode substrate, wherein the first electrode and the second electrode are gold electrodes;
(3) taking 1.0-10.0 microliters of the molybdenum disulfide-doped nano silver particle composite dispersion liquid obtained in the step (1), attaching the dispersion liquid to the surface of the electrode substrate obtained in the step (2) by using a coating method, and then placing the electrode substrate into protective gas at the temperature of not higher than 50 ℃ for standing for 1-2 hours for drying treatment, thereby obtaining the electrode substrate with a layer of molybdenum disulfide-doped nano silver particle composite film attached to the surface;
(4) and (4) measuring the humidity by measuring the capacitance change between the first electrode and the second electrode of the electrode substrate which is obtained in the step (3) and is attached with a layer of molybdenum disulfide doped nano silver particle composite material film on the surface.
In the step (1), the volume ratio of the doped nano silver particle aqueous dispersion to the doped molybdenum disulfide aqueous dispersion is more than 1:5, due to the seepage threshold effect, the basic capacitance of the prepared sensor is lowered in a cliff manner, and the sensor cannot be used. When the volume ratio of the doped nano silver particle aqueous dispersion to the doped molybdenum disulfide aqueous dispersion is less than 1: at 20, the silver particle ratio is too small, and the sensitivity of the sensor is improved only to a limited extent.
Preferably, the vacuum coating method in the step (2) is an evaporation coating method or a sputter coating method.
Preferably, the coating method in the step (3) is one of a dropping method, a spin coating method or a spray coating method.
Preferably, the protective gas in step (3) is nitrogen.
In order to achieve the purpose, the invention provides a molybdenum disulfide doped nano silver particle composite humidity sensor which is prepared by any one of the methods.
Preferably, the composite humidity sensor includes: the composite material comprises a silicon substrate at the bottom, a silicon dioxide layer above the silicon substrate, a first electrode and a second electrode on the surface of the silicon dioxide layer, and a molybdenum disulfide doped nano silver particle composite material film between the first electrode and the second electrode and on the upper surface.
Preferably, the electrode patterns in the electrode substrate are comb-shaped and staggered, that is, a second electrode is arranged between adjacent first electrodes, and a first electrode is arranged between adjacent second electrodes.
The invention has the beneficial effects that: the humidity sensor provided by the invention adopts the molybdenum disulfide-doped nano silver particle composite material film as the humidity sensitive medium, and the nano silver particles with the particle size of less than or equal to 100 nanometers are doped into the molybdenum disulfide material, so that the adsorption sites of water molecules are increased, the adsorption of the water molecules on the surface and in the sensitive medium and the formation of a liquid water layer are facilitated, the specific surface area of the sensitive film material can be increased, and the humidity sensor has higher response sensitivity and higher response speed due to the reasons.
Drawings
FIG. 1 is a cross-sectional view of a molybdenum disulfide doped nano silver particle composite humidity sensor of the present invention;
FIG. 2 is a top view of an electrode structure of the molybdenum disulfide doped nano silver particle composite humidity sensor of the present invention;
FIG. 3 is a top view of the molybdenum disulfide doped nano silver particle composite humidity sensor of the present invention;
FIG. 4 is a graph of humidity-sensitive response capacitance data for a molybdenum disulfide doped nano-silver particle composite humidity sensor of the present invention;
FIG. 5 is a graph of humidity-sensitive response time data for the molybdenum disulfide doped nano-silver particle composite humidity sensor of the present invention.
The material comprises a substrate 1, a silicon dioxide layer 2, a first electrode 3, a second electrode 4, a molybdenum disulfide-doped nano silver particle composite material film 5, a molybdenum disulfide nanosheet 51 and nano silver particles 52.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Example 1
A preparation method of a molybdenum disulfide doped nano silver particle composite humidity sensor comprises the following steps:
(1) doping nano silver particles with the particle size of less than or equal to 100 nanometers into water to form nano silver particle aqueous dispersion with the concentration of 0.1 mg/ml, doping the nano silver particle aqueous dispersion into molybdenum disulfide aqueous dispersion with the concentration of 0.1 mg/ml, wherein the volume ratios of the doped molybdenum disulfide aqueous dispersion and the nano silver particle aqueous dispersion are respectively 5:1, 10:1, 15:1 and 20:1, obtaining 4 samples, and performing ultrasonic dispersion for 2 hours to obtain molybdenum disulfide-doped nano silver particle composite dispersion;
(2) cleaning a silicon substrate, forming a silicon dioxide layer on the surface of the silicon substrate by using a thermal oxidation method, and then forming a first electrode and a second electrode on the surface of the silicon dioxide layer by using a vacuum coating method to obtain an electrode substrate, wherein the first electrode and the second electrode are gold electrodes;
(3) taking 1.0 microliter of the molybdenum disulfide-doped nano silver particle composite dispersion liquid obtained in the step (1), attaching the dispersion liquid to the surface of the electrode substrate obtained in the step (2) by using a coating method, and then placing the electrode substrate in protective gas at the temperature of not higher than 50 ℃ for standing for 1 hour for drying treatment, thereby obtaining the electrode substrate with a layer of molybdenum disulfide-doped nano silver particle composite film attached to the surface;
(4) and (4) measuring the humidity by measuring the capacitance change between the first electrode and the second electrode of the electrode substrate which is obtained in the step (3) and is attached with a layer of molybdenum disulfide doped nano silver particle composite material film on the surface.
Specifically, the vacuum coating method in the step (2) is an evaporation coating method.
Specifically, the coating method in step (3) is a drop coating method.
Specifically, the protective gas in step (3) is nitrogen.
As shown in fig. 1 and fig. 3, the molybdenum disulfide-doped nano silver particle composite humidity sensor prepared by the method includes: the composite material film comprises a silicon substrate 1 at the bottom, a silicon dioxide layer 2 above the silicon substrate 1, a first electrode 3 and a second electrode 4 on the surface of the silicon dioxide layer 2, a molybdenum disulfide-doped nano silver particle composite material film 5 between the first electrode 3 and the second electrode 4 and on the upper surface, and molybdenum disulfide nanosheets 51 and nano silver particles 52 in the molybdenum disulfide-doped nano silver particle composite material film 5.
As shown in fig. 2, the electrode patterns in the electrode substrate are comb-shaped and staggered, that is, a second electrode is disposed between adjacent first electrodes, and a first electrode is disposed between adjacent second electrodes.
Example 2
A preparation method of a molybdenum disulfide doped nano silver particle composite humidity sensor comprises the following steps:
(1) doping nano silver particles with the particle size of less than or equal to 100 nanometers into water to form nano silver particle aqueous dispersion with the concentration of 4.0 mg/ml, doping the nano silver particle aqueous dispersion into molybdenum disulfide aqueous dispersion with the concentration of 4.0 mg/ml, wherein the volume ratios of the doped molybdenum disulfide aqueous dispersion and the nano silver particle aqueous dispersion are respectively 5:1, 10:1, 15:1 and 20:1, obtaining 4 samples, and performing ultrasonic dispersion for 24 hours to obtain molybdenum disulfide-doped nano silver particle composite dispersion;
(2) cleaning a silicon substrate, forming a silicon dioxide layer on the surface of the silicon substrate by using a thermal oxidation method, and then forming a first electrode and a second electrode on the surface of the silicon dioxide layer by using a vacuum coating method to obtain an electrode substrate, wherein the first electrode and the second electrode are gold electrodes;
(3) taking 10.0 microliter of the molybdenum disulfide-doped nano silver particle composite dispersion liquid obtained in the step (1), attaching the dispersion liquid to the surface of the electrode substrate obtained in the step (2) by using a coating method, and then placing the electrode substrate into protective gas at the temperature of not higher than 50 ℃ for standing for 2 hours for drying treatment, thereby obtaining the electrode substrate with a layer of molybdenum disulfide-doped nano silver particle composite film attached to the surface;
(4) and (4) measuring the humidity by measuring the capacitance change between the first electrode and the second electrode of the electrode substrate which is obtained in the step (3) and is attached with a layer of molybdenum disulfide doped nano silver particle composite material film on the surface.
Specifically, the vacuum coating method in the step (2) is a sputter coating method.
Specifically, the coating method in step (3) is a spin coating method.
Specifically, the protective gas in step (3) is nitrogen.
As shown in fig. 1 and fig. 3, the molybdenum disulfide-doped nano silver particle composite humidity sensor prepared by the method includes: the composite material film comprises a silicon substrate 1 at the bottom, a silicon dioxide layer 2 above the silicon substrate 1, a first electrode 3 and a second electrode 4 on the surface of the silicon dioxide layer 2, a molybdenum disulfide-doped nano silver particle composite material film 5 between the first electrode 3 and the second electrode 4 and on the upper surface, and molybdenum disulfide nanosheets 51 and nano silver particles 52 in the molybdenum disulfide-doped nano silver particle composite material film 5.
As shown in fig. 2, the electrode patterns in the electrode substrate are comb-shaped and staggered, that is, a second electrode is disposed between adjacent first electrodes, and a first electrode is disposed between adjacent second electrodes.
Example 3
A preparation method of a molybdenum disulfide doped nano silver particle composite humidity sensor comprises the following steps:
(1) adding nano silver particles with the particle size of less than or equal to 100 nanometers into water to form nano silver particle aqueous dispersion with the concentration of 2 mg/ml, adding the nano silver particle aqueous dispersion into molybdenum disulfide aqueous dispersion with the concentration of 2 mg/ml, wherein the volume ratios of the added molybdenum disulfide aqueous dispersion and the nano silver particle aqueous dispersion are respectively 5:1, 10:1, 15:1 and 20:1, obtaining 4 samples, and performing ultrasonic dispersion for 13 hours to obtain molybdenum disulfide-doped nano silver particle composite material dispersion;
(2) cleaning a silicon substrate, forming a silicon dioxide layer on the surface of the silicon substrate by using a thermal oxidation method, and then forming a first electrode and a second electrode on the surface of the silicon dioxide layer by using a vacuum coating method to obtain an electrode substrate, wherein the first electrode and the second electrode are gold electrodes;
(3) taking 6 microliters of the molybdenum disulfide-doped nano silver particle composite dispersion liquid obtained in the step (1), attaching the dispersion liquid to the surface of the electrode substrate obtained in the step (2) by using a coating method, and then placing the electrode substrate in protective gas at a temperature of not higher than 50 ℃ for standing for 1.5 hours for drying treatment, thereby obtaining the electrode substrate with a layer of molybdenum disulfide-doped nano silver particle composite film attached to the surface;
(4) and (4) measuring the humidity by measuring the capacitance change between the first electrode and the second electrode of the electrode substrate which is obtained in the step (3) and is attached with a layer of molybdenum disulfide doped nano silver particle composite material film on the surface.
Specifically, the vacuum coating method in the step (2) is an evaporation coating method.
Specifically, the coating method in the step (3) is a spray coating method.
Specifically, the protective gas in step (3) is nitrogen.
As shown in fig. 1 and fig. 3, the molybdenum disulfide-doped nano silver particle composite humidity sensor prepared by the method includes: the composite material film comprises a silicon substrate 1 at the bottom, a silicon dioxide layer 2 above the silicon substrate 1, a first electrode 3 and a second electrode 4 on the surface of the silicon dioxide layer 2, a molybdenum disulfide-doped nano silver particle composite material film 5 between the first electrode 3 and the second electrode 4 and on the upper surface, and molybdenum disulfide nanosheets 51 and nano silver particles 52 in the molybdenum disulfide-doped nano silver particle composite material film 5.
As shown in fig. 2, the electrode patterns in the electrode substrate are comb-shaped and staggered, that is, a second electrode is disposed between adjacent first electrodes, and a first electrode is disposed between adjacent second electrodes.
Performance analysis
FIG. 4 is a graph of humidity-sensitive response capacitance data for a molybdenum disulfide doped nano-silver particle composite humidity sensor of the present invention; as shown in fig. 4, the capacitance humidity-sensitive response of the prepared molybdenum disulfide-doped silver nanoparticle composite sensor increases with the increase of the volume ratio of the molybdenum disulfide dispersion to the silver nanoparticle dispersion, and the humidity-sensitive response capacitance value of the sensor is improved by more than 22 times compared with the sensor prepared by coating the sensor with pure molybdenum disulfide dispersion with the same volume and the same concentration. And (2) in different samples obtained in the step (1), the performance is optimal when the volume ratio of the doped nano silver particle aqueous dispersion to the doped molybdenum disulfide aqueous dispersion is 1: 5. In the step (1), the volume ratio of the doped nano silver particle aqueous dispersion to the doped molybdenum disulfide aqueous dispersion is more than 1:5, due to the seepage threshold effect, the basic capacitance of the prepared sensor is lowered in a cliff manner, and the sensor cannot be used. When the volume ratio of the doped nano silver particle aqueous dispersion to the doped molybdenum disulfide aqueous dispersion is less than 1: at 20, the silver particle ratio is too small, and the sensitivity of the sensor is improved only to a limited extent.
FIG. 5 is a graph of humidity-sensitive response time data for the molybdenum disulfide doped nano-silver particle composite humidity sensor of the present invention. The ordinate represents capacitance and the abscissa represents response time, wherein the percentage represents relative humidity. As shown in FIG. 5, The response time of The composite sensor of molybdenum disulfide doped with nano silver particles prepared by The above method is less than or equal to 2 seconds, and The response speed is greatly improved compared with that of a capacitive relative humidity sensor based on pure molybdenum disulfide mentioned in The combinations of hole MoS2 micro @ nanospheres, one-step synthesis, excellent photocatalytic and humidity sensing properties.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (7)
1. A preparation method of a molybdenum disulfide doped nano silver particle composite humidity sensor is characterized by comprising the following steps:
(1) doping nano silver particles with the particle size of less than or equal to 100 nanometers into water to form nano silver particle aqueous dispersion with the concentration of 0.1-4.0 mg/ml, doping the nano silver particle aqueous dispersion into molybdenum disulfide aqueous dispersion with the concentration of 0.1-4.0 mg/ml, wherein the volume ratio of the doped nano silver particle aqueous dispersion to the doped molybdenum disulfide aqueous dispersion is less than or equal to 1:5 and more than or equal to 1:20, and performing ultrasonic dispersion for 2-24 hours to obtain molybdenum disulfide-doped nano silver particle composite dispersion;
(2) cleaning a silicon substrate, forming a silicon dioxide layer on the surface of the silicon substrate by using a thermal oxidation method, and then forming a first electrode and a second electrode on the surface of the silicon dioxide layer by using a vacuum coating method to obtain an electrode substrate, wherein the first electrode and the second electrode are gold electrodes;
(3) taking 1.0-10.0 microliters of the molybdenum disulfide-doped nano silver particle composite dispersion liquid obtained in the step (1), attaching the dispersion liquid to the surface of the electrode substrate obtained in the step (2) by using a coating method, and then placing the electrode substrate into protective gas at the temperature of not higher than 50 ℃ for standing for 1-2 hours for drying treatment, thereby obtaining the electrode substrate with a layer of molybdenum disulfide-doped nano silver particle composite film attached to the surface;
(4) and (4) measuring the humidity by measuring the capacitance change between the first electrode and the second electrode of the electrode substrate which is obtained in the step (3) and is attached with a layer of molybdenum disulfide doped nano silver particle composite material film on the surface.
2. The method for preparing the molybdenum disulfide doped nano silver particle composite humidity sensor according to claim 1, wherein the molybdenum disulfide doped nano silver particle composite humidity sensor comprises the following steps: the vacuum coating method in the step (2) is an evaporation coating method or a sputtering coating method.
3. The method for preparing the molybdenum disulfide doped nano silver particle composite humidity sensor according to claim 1, wherein the molybdenum disulfide doped nano silver particle composite humidity sensor comprises the following steps: the coating method in the step (3) is one of a dropping coating method, a spin coating method or a spraying coating method.
4. The method for preparing the molybdenum disulfide doped nano silver particle composite humidity sensor according to claim 1, wherein the molybdenum disulfide doped nano silver particle composite humidity sensor comprises the following steps: and (4) adopting nitrogen as the protective gas in the step (3).
5. The molybdenum disulfide-doped nano silver particle composite humidity sensor is characterized in that: which is prepared by the method of any one of claims 1 to 4.
6. The molybdenum disulfide doped nano silver particle composite humidity sensor according to claim 5, comprising: the composite material comprises a silicon substrate at the bottom, a silicon dioxide layer above the silicon substrate, a first electrode and a second electrode on the surface of the silicon dioxide layer, and a molybdenum disulfide doped nano silver particle composite material film between the first electrode and the second electrode and on the upper surface.
7. The molybdenum disulfide doped nano silver particle composite humidity sensor according to claim 6, wherein: the electrode patterns in the electrode substrate are comb-tooth-shaped and staggered, namely, a second electrode is arranged between the adjacent first electrodes, and a first electrode is arranged between the adjacent second electrodes.
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| CN108169284B (en) * | 2017-12-14 | 2021-01-01 | 上海交通大学 | Humidity sensor based on carbon dot doped molybdenum disulfide sheet 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 |
| 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 |
| 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 |
| 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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