CN106124574B - Graphene oxide quantum dot humidity sensor and preparation method thereof - Google Patents
Graphene oxide quantum dot humidity sensor and preparation method thereof Download PDFInfo
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- CN106124574B CN106124574B CN201610443637.7A CN201610443637A CN106124574B CN 106124574 B CN106124574 B CN 106124574B CN 201610443637 A CN201610443637 A CN 201610443637A CN 106124574 B CN106124574 B CN 106124574B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/121—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid for determining moisture content, e.g. humidity, of the fluid
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
Abstract
The present invention provides a kind of graphene oxide quantum dot humidity sensor and preparation method thereof, and sensor includes: silicon chip, silicon dioxide layer, first electrode and second electrode, diallyl dimethyl ammoniumchloride film, graphene oxide quantum dot film；Preparation method is the following steps are included: (1) forms layer of silicon dioxide layer in silicon substrate surface, first electrode and second electrode are formed in silica layer surface, obtain electrode base sheet, (2) between the first electrode and the second electrode and its surface electrostatic adsorb a strata diallyldimethylammonium chloride film, (3) in one layer of graphene oxide quantum dot film of diallyl dimethyl ammoniumchloride film surface Electrostatic Absorption, humidity sensor of the invention has the response speed being exceedingly fast, resistance to high humidity corrodes, and anti-electromagnetic interference capability is strong.
Description
Technical field
The present invention relates to sensor manufacturing fields, are related specifically to a kind of with super fast response, the erosion of resistance to high humidity, anti-electromagnetism
Graphene oxide quantum dot humidity sensor of the characteristics of interference and preparation method thereof.
Background technique
Often there is humidity sensor in the fields such as unmanned plane meteorological detection, sounding balloon, the monitoring of gas drilling formation water output
Higher application requirement, the humidity sensor in these fields should have ultrafast response speed, have preferable resistance to height again
Wet erosion performance, while also needing that there is good electromagnetism interference characteristic, therefore the high performance humidity sensor of exploitation has ten
Divide important meaning.
2015, document Subsecond Response of Humidity Sensor Based on Graphene
A kind of impedance type humidity sensor based on graphene oxide quantum dot, the sensor are proposed in Oxide Quantum Dots
Electrode unit is plane interdigitated structure, and graphene oxide quantum dot dispersion liquid is spin-coated on electrode zone, this humidity sensor
Using graphene oxide quantum dot as humidity sensitive material, graphene oxide quantum dot has very big specific surface area and rich
Rich hydrophilic radical, which can reach the response speed of submicrosecond grade, but the thin film-forming method of spin coating causes humidity sensitive
The thickness of film is thicker and the adhesion of film and substrate is poor, therefore the response speed of this sensor is difficult to further increase, and
And vulnerable to extraneous moisture attacks, sensor performance is influenced.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide one kind there is super fast response, resistance to high humidity to corrode, is anti-
The electric resistance moisture sensor of graphene oxide quantum dot and preparation method thereof of the strong feature of electromagnetic interference capability.
For achieving the above object, technical solution of the present invention is as follows:
A kind of preparation method of graphene oxide quantum dot humidity sensor, comprising the following steps:
(1) silicon chip is cleaned up, forms layer of silicon dioxide layer in silicon substrate surface, is then existed with Vacuum Coating method
Silica layer surface forms spacing and is less than or equal to 20 microns of first electrode and second electrode, obtains electrode base sheet, and described the
One electrode and second electrode are gold electrode；Spacing is set to be the response speed in order to improve electrode less than or equal to 20 microns.
(2) electrode base sheet obtained in step (1) is immersed into the polydiene propyl two that concentration is 0.2~2.0 mg/ml
Ammonio methacrylate aqueous solution soaking 5~15 minutes, between the first electrode and the second electrode and its adsorption by electrostatic force
One strata diallyldimethylammonium chloride film, which is transferred in deionized water and is rinsed 1~30 minute, removal
Fall the diallyl dimethyl ammoniumchloride for not being securely attached between first electrode and second electrode and its surface, then should
Electrode base sheet after rinsing, which is placed into, to be stood 1~2 hour in the protective gas not higher than 50 DEG C and is dried, to obtain
Surface is attached with the electrode base sheet of a strata diallyldimethylammonium chloride film；
(3) surface obtained in step (2) is attached with to the electrode base of a strata diallyldimethylammonium chloride film
It is to soak in the graphene oxide quantum dot dispersion liquid of 0.5~2.0 mg/ml and partial size less than or equal to 20 nanometers that piece, which immerses concentration,
Bubble 5~15 minutes adsorbs one layer of graphene oxide quantum in diallyl dimethyl ammoniumchloride film surface by electrostatic force
Point film, which, which is transferred to deionized water, rinses 1~30 minute, gets rid of and is not adsorbed onto polydiene propyl two securely
Then the electrode base sheet after rinsing is placed into not higher than 50 DEG C by the graphene oxide quantum dot of ammonio methacrylate film surface
Protective gas in stand 1~2 hour and be dried, have one layer of graphene oxide quantum dot thin to obtain adsorption
The electrode base sheet of film；Setting graphene oxide quantum dot partial size be less than or equal to 20 nanometers be with are as follows: the smaller surface area of partial size is got over
Greatly, more hydrones can be adsorbed in this way, to improve the response speed of sensor.
(4) there is the electrode base of one layer of graphene oxide quantum dot film by adsorption obtained in measuring process (3)
Resistance variations between the first electrode and second electrode of piece measure humidity.
It is preferred that the Vacuum Coating method in step (1) is evaporation or sputtering method.
It is preferred that step (1) middle thermal oxidation method forms layer of silicon dioxide layer in silicon substrate surface.
It is preferred that the protective gas in step (2) and step (3) is nitrogen.
The present invention also provides a kind of graphene oxide quantum dot humidity sensors, comprising: on the silicon chip of bottom, silicon chip
The silicon dioxide layer of side, between the first electrode of silica layer surface and second electrode, first electrode and second electrode and on
The diallyl dimethyl ammoniumchloride film on surface, diallyl dimethyl ammoniumchloride film upper surface graphene oxide
Quantum dot film.
It is preferred that electrode pattern is comb teeth-shaped and is staggered in the electrode base sheet, i.e., the first adjacent electricity
It is equipped with second electrode between pole, is equipped with first electrode between adjacent second electrode.
It is preferred that the humidity sensor is prepared using any one of the above the method.
The invention has the benefit that humidity sensor proposed by the present invention uses graphene oxide quantum dot and polydiene
Diallyidimethylammonium chloride duplicature has as humidity sensitive medium, graphene oxide quantum dot of the partial size less than or equal to 20 nanometers
There are very big specific surface area and hydrophilic functional groups abundant；The polydiene propyl removed Xi Fu loosely is rinsed by deionized water
Very thin humidity sensitive film can be obtained in alkyl dimethyl ammonium chloride and graphene oxide quantum dot, so that water molecule energy use is shorter
Time spreads from sensitive membrane upper surface reaches bottom；Electrode spacing is less than or equal to be 20 microns simultaneously, can make between electrode
Sensitive membrane width it is smaller, be conducive to electronics conduction.The above reason causes the humidity sensor to have the response speed being exceedingly fast
Degree.Secondly, diallyl dimethyl ammoniumchloride and graphene oxide quantum dot are adsorbed onto first electrode by electrostatic force
Between second electrode and surface, and rinsed by deionized water the diallyl dimethyl ammoniumchloride removed Xi Fu loosely with
Graphene oxide quantum dot, therefore the diallyl dimethyl ammoniumchloride removed and graphite oxide are not rinsed by deionized water
The characteristic that there is alkene quantum dot tolerance high humidity to corrode.In addition, sensor passes through the electricity between measurement first electrode and second electrode
Resistive measures humidity, relative to capacitance type humidity sensor, has stronger anti-electromagnetic interference capability.
Detailed description of the invention
Fig. 1 is the sectional view of graphene oxide quantum dot humidity sensor of the invention；
Fig. 2 is the electrode structure top view of graphene oxide quantum dot humidity sensor of the invention；
Fig. 3 is the top view of graphene oxide quantum dot humidity sensor of the invention；
Wherein, 1 is silicon chip, and 2 be silicon dioxide layer, and 3 be first electrode, and 4 be second electrode, and 5 be polydiene propyl two
Ammonio methacrylate film, 6 be graphene oxide quantum dot film.
Specific embodiment
Illustrate embodiments of the present invention below by way of specific specific example, those skilled in the art can be by this specification
Other advantages and efficacy of the present invention can be easily understood for disclosed content.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints and application, without departing from
Various modifications or alterations are carried out under spirit of the invention.
A kind of preparation method of graphene oxide quantum dot humidity sensor, comprising the following steps:
(1), silicon chip is cleaned up, forms layer of silicon dioxide layer in silicon substrate surface thermal oxidation method, then uses
Vacuum Coating method forms the first electrode and second electrode that spacing is less than or equal to 20 microns in silica layer surface, obtains electrode
Substrate, the first electrode and second electrode are gold electrode；It is to improve electrode that setting spacing, which is less than equal to 20 microns,
Response speed.
(2), electrode base sheet obtained in step (1) is immersed into the polydiene propyl that concentration is 0.2~2.0 mg/ml
Alkyl dimethyl ammonium chloride aqueous solution soaking 5~15 minutes, by electrostatic force between the first electrode and the second electrode and its surface inhale
Attached strata diallyldimethylammonium chloride film, which is transferred in deionized water and is rinsed 1~30 minute, is gone
The diallyl dimethyl ammoniumchloride for not being securely attached between first electrode and second electrode and its surface is removed, then will
The electrode base sheet after rinsing, which is placed into, to be stood 1~2 hour in the nitrogen not higher than 50 DEG C and is dried, to obtain table
Face is attached with the electrode base sheet of a strata diallyldimethylammonium chloride film；
(3), surface obtained in step (2) is attached with to the electrode base of a strata diallyldimethylammonium chloride film
It is to soak in the graphene oxide quantum dot dispersion liquid of 0.5~2.0 mg/ml and partial size less than or equal to 20 nanometers that piece, which immerses concentration,
Bubble 5~15 minutes adsorbs one layer of graphene oxide quantum in diallyl dimethyl ammoniumchloride film surface by electrostatic force
Point film, which, which is transferred to deionized water, rinses 1~30 minute, gets rid of and is not adsorbed onto polydiene propyl two securely
Then the electrode base sheet after rinsing is placed into not higher than 50 DEG C by the graphene oxide quantum dot of ammonio methacrylate film surface
Nitrogen in stand 1~2 hour and be dried, so that obtaining adsorption has one layer of graphene oxide quantum dot film
Electrode base sheet；Setting graphene oxide quantum dot partial size be less than or equal to 20 nanometers be with are as follows: the smaller surface area of partial size is bigger, this
Sample can adsorb more hydrones, to improve the response speed of sensor.
(4), there is the electrode base of one layer of graphene oxide quantum dot film by adsorption obtained in measuring process (3)
Resistance variations between the first electrode and second electrode of piece measure humidity.
Vacuum Coating method in step (1) is evaporation or sputtering method.
As shown in Figure 1, Figure 3, a kind of graphene oxide quantum dot humidity sensor prepared using the above method, comprising:
The silicon chip 1 of bottom, 1 top of silicon chip silicon dioxide layer 2, the first electrode 3 on 2 surface of silicon dioxide layer and second electrode 4,
Diallyl dimethyl ammoniumchloride film 5, the polydiene dimethylamine of between first electrode 3 and second electrode 4 and upper surface
The graphene oxide quantum dot film 6 of 5 upper surface of ammonium chloride film.
As shown in Fig. 2, electrode pattern is comb teeth-shaped and to be staggered in the electrode base sheet, i.e., adjacent first electrode it
Between be equipped with second electrode, first electrode is equipped between adjacent second electrode.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, all those of ordinary skill in the art are completed without departing from the spirit and technical ideas disclosed in the present invention
All equivalent modifications or change, should be covered by the claims of the present invention.
Claims (6)
1. a kind of preparation method of graphene oxide quantum dot humidity sensor, it is characterised in that the following steps are included:
(1) silicon chip is cleaned up, layer of silicon dioxide layer is formed in silicon substrate surface, then with Vacuum Coating method in dioxy
SiClx layer surface forms the first electrode and second electrode that spacing is less than or equal to 20 microns, obtains electrode base sheet, first electricity
Pole and second electrode are gold electrode；
(2) electrode base sheet obtained in step (1) is immersed into the diallyl dimethyl that concentration is 0.2~2.0 mg/ml
Aqueous ammonium chloride solution impregnates 5~15 minutes, between the first electrode and the second electrode and its one layer of adsorption by electrostatic force
The electrode base sheet is transferred in deionized water and rinses 1~30 minute, gets rid of not by diallyl dimethyl ammoniumchloride film
It is securely attached to the diallyl dimethyl ammoniumchloride between first electrode and second electrode and its surface, then rinses this
Electrode base sheet afterwards, which is placed into, to be stood 1~2 hour in the protective gas not higher than 50 DEG C and is dried, to obtain surface
It is attached with the electrode base sheet of a strata diallyldimethylammonium chloride film；
(3) electrode base sheet that surface obtained in step (2) is attached with a strata diallyldimethylammonium chloride film is soaked
Entering concentration is to impregnate 5 in the graphene oxide quantum dot dispersion liquid of 0.5~2.0 mg/ml and partial size less than or equal to 20 nanometers
It is~15 minutes, thin in diallyl dimethyl ammoniumchloride film surface one layer of graphene oxide quantum dot of absorption by electrostatic force
The electrode base sheet is transferred to deionized water and rinsed 1~30 minute, got rid of and be not adsorbed onto diallyl dimethyl securely by film
Then the electrode base sheet after rinsing is placed into the guarantor not higher than 50 DEG C by the graphene oxide quantum dot on ammonium chloride film surface
It stands 1~2 hour in shield gas to be dried, so that obtaining adsorption has one layer of graphene oxide quantum dot film
Electrode base sheet；
(4) there is the electrode base sheet of one layer of graphene oxide quantum dot film by adsorption obtained in measuring process (3)
Resistance variations between first electrode and second electrode measure humidity.
2. the preparation method of graphene oxide quantum dot humidity sensor according to claim 1, it is characterised in that: step
(1) Vacuum Coating method in is evaporation or sputtering method.
3. the preparation method of graphene oxide quantum dot humidity sensor according to claim 1, it is characterised in that: step
(1) middle thermal oxidation method forms layer of silicon dioxide layer in silicon substrate surface.
4. the preparation method of graphene oxide quantum dot humidity sensor according to claim 1, it is characterised in that: step
(2) protective gas and in step (3) is nitrogen.
5. a kind of graphene oxide quantum dot humidity sensor, it is characterised in that: using described in Claims 1-4 any one
Preparation method obtains, comprising: the first electricity of silicon dioxide layer, silica layer surface above the silicon chip of bottom, silicon chip
The diallyl dimethyl ammoniumchloride film of between pole and second electrode, first electrode and second electrode and upper surface, poly- two
The graphene oxide quantum dot film of allyl dimethyl ammonium chloride film upper surface.
6. graphene oxide quantum dot humidity sensor according to claim 5, it is characterised in that: in the electrode base sheet
Electrode pattern is comb teeth-shaped and to be staggered, i.e., is equipped with second electrode between adjacent first electrode, adjacent second electrode it
Between be equipped with first electrode.
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| JP6770238B2 (en) * | 2017-03-31 | 2020-10-14 | ミツミ電機株式会社 | Humidity sensor |
| CN107064242B (en) * | 2017-04-11 | 2020-01-17 | 西南交通大学 | Molybdenum disulfide doped nano silver particle composite humidity sensor and preparation method thereof |
| CN106946212A (en) * | 2017-05-08 | 2017-07-14 | 河南理工大学 | A kind of surface quantum point humidity sensor chip |
| CN108896623B (en) * | 2018-07-11 | 2020-01-31 | 西南交通大学 | digital frequency type humidity sensor for measuring relative humidity of gas |
| CN108982415B (en) * | 2018-08-14 | 2020-03-24 | 东北大学 | GQDs-PVA filling-based FPI cascaded optical fiber humidity sensor 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 |
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