CN105699441B - A kind of resistance-type gas sensor and preparation method thereof - Google Patents
A kind of resistance-type gas sensor and preparation method thereof Download PDFInfo
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- CN105699441B CN105699441B CN201610172151.4A CN201610172151A CN105699441B CN 105699441 B CN105699441 B CN 105699441B CN 201610172151 A CN201610172151 A CN 201610172151A CN 105699441 B CN105699441 B CN 105699441B
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- gas
- interdigital electrode
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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
Abstract
The present invention provides a kind of resistance-type gas sensor and preparation method thereof, the invention belongs to gas sensor technical field.The resistance-type gas sensor of the present invention, including dielectric substrate, interdigital electrode and gas sensing layer；The gas sensing layer is divided into two symmetrical subregions using the center line of interdigital electrode as symmetry axis in insulated substrate surface, and each subregion deposits the gas-sensitive film layer for having different responses to same specific gas respectively.The method comprises the steps of firstly, preparing go out insulating layer, interdigital electrode negative patterning is lithographically formed in insulating layer afterwards, deposits suitable interdigital electrode, it is divided into two symmetrical regions by symmetry axis of the center line of interdigital electrode again, the gas-sensitive film layer that there are different responses to same specific gas is finally deposited in each subregion, the resistance-type gas sensor is made.Production cost of the present invention is low, technique is simple；Improve the selectivity to specific gas；The influence that baseline drift detects gas can be improved at the same time, improve the stability and measurement accuracy of gas sensor.
Description
Technical field
The present invention relates to gas sensor technical field, and in particular to a kind of resistance-type gas sensor and its preparation side
Method.
Background technology
Gas sensor is the core of gas detecting system, is that certain gas volume fraction is changed into corresponding telecommunications by one kind
Number device.Gas sensor be by generation adsorption or reaction when interact with gas, cause sensor conductance rate,
The change of sole mass or other characteristics, so as to detect the concentration of tested gas.Wherein, Gas Sensors of Electric Resistance Semiconductors
It is a common type in gas sensor, it is more is widely used in industry, chemical industry, electronics, electric power, lathe, oil etc.
In a field.
Resistor-type gas sensor is by caused resistance variations when gas absorption and reaction come detection gas.Resistance-type gas
In body sensor it is particularly important that sensitive membrane material, in gas sensor, since sensitive membrane of the same race has multiple gases necessarily
The response of degree, is only difficult to realize efficient identification and Concentration Testing to heterogeneity gas by single sensitive membrane.
Common method is to take composite membrane, multilayer film and multilayer complex films in terms of gas-selectively is improved both at home and abroad at present
Three kinds of modes.Composite membrane is to mix a variety of gas sensitives according to special ratios, is then coated with forming a film in device surface；Multilayer film
It is that a variety of gas sensitives successively form a film according to certain order coated on device surface；Multilayer complex films are then by compound gas
Quick material successively forms a film according to certain order coated on device surface.These types of pattern has its advantage, but scarce there is also it
Point：The gas sensitive of composite membrane mixes, and gas-sensitive property may change, and deviates default response results；Multilayer film
Internal layer membrane may be not easy to contact gas molecule, reduce responsiveness and selectivity, and to easily lead to desorption incomplete for multilayer film,
Cause baseline drift；In order to reach higher response and preferable selectivity, composite membrane and multilayer film are in formulation selection and processing
Process aspect is more demanding, and flow is complicated, and processing difficulties degree is big.Therefore it provides a kind of simple possible, new gas sensing
Device sensitive thin film structure and preparation method solve the problems, such as that conventional composite, multi-layer sensitive film exist, and then improve gas sensing
The performance of device is very necessary.
The content of the invention
It is an object of the present invention to provide a kind of resistance-type gas sensor and preparation method thereof；The present invention can solve
Resistance sensor gas sensitive based on sensitive membrane gas absorption is selectively bad and conventional composite, multi-layer sensitive film solution
Caused by absorption not exclusively the shortcomings that baseline drift, selectivity, stability and the measurement accuracy of enhancing gas sensor detection.
Technical scheme is as follows：
A kind of resistance-type gas sensor, it is characterised in that the interdigital electrode including dielectric substrate, in dielectric substrate
And it is deposited on the gas-sensitive film layer in interdigital electrode；The gas-sensitive film layer is with the symmetrical central axes of interdigital electrode
Two symmetrical subregions are divided into device surface for symmetry axis, each subregion has deposited respectively has same specific gas
There is the gas-sensitive film layer of different responses.
Wherein, the interdigital electrode material is gold or aluminium, and interdigital electrode logarithm is 10~15 pairs, and it is 10~100 μ to refer to spacing
m。
A kind of preparation method of resistance-type gas sensor, comprises the following steps：
Step 1：Substrate is cleaned and is pre-processed, one layer uniform two is grown in substrate surface by thermal oxidation method
Insulating layer of silicon oxide；
Step 2：Interdigital electrode logarithm is lithographically formed on silicon dioxide insulating layer as 10~15 pairs, refer to spacing for 10~
100 μm of interdigital electrode negative patterning；
Step 3:Sputtering forms nickel-chrome alloy layer on the interdigital electrode negative patterning obtained by step 2, then in nickel chromium triangle layer surface
Gold plated Layer or aluminium lamination, finally remove unnecessary layer gold or aluminium lamination, obtain interdigital electrode；
Step 4：Using the symmetrical central axes of interdigital electrode as symmetry axis two symmetrical subregions, institute are formed in device surface
It is the gas-sensitive film layer for having different responses to same specific gas to state each subregion, so that resistance-type gas sensing be made
Device.
The cleaning of substrate and the adhesion and subsequent process flow of film of the pretreatment to growth thereon in the step 1
Influence is very big, therefore needs substrate to clean up in step 1.Glass substrate is typically chosen, common cleaning method can
To be soaked in the mixed solution of the concentrated sulfuric acid and hydrogen peroxide, the organic pollution being attached in glass substrate is removed；Then put again
Enter and be cleaned by ultrasonic respectively in the alkaline solutions such as ammonium hydroxide, hydrochloric acid solution, acetone soln, ethanol solution, it is dirty to remove metal ion
Dye and particle contamination；Substrate surface moisture finally is blown away with the nitrogen of dried and clean, it is fully dry in drying box；
The step 2 uses Ultraviolet lithography, first with sol evenning machine in one layer of uniform photoetching of surface of insulating layer spin coating
Glue, is exposed using positive mask plate on deep UV lithography machine, and then development obtains mask graph in developer solution, is lithographically formed conjunction
Suitable interdigital electrode negative patterning；
In the step 3, on the good interdigital electrode negative patterning of photoetching with the method for magnetron sputtering sputtering thickness for 5~
The nickel-chrome alloy layer of 10nm to improve the adhesion of device surface, and nickel chromium triangle layer surface use vacuum vapour deposition evaporation thickness for
The layer gold or aluminium lamination of 50~100nm, can be heat-treated to strengthen nicr layer and layer gold or the adhesion of aluminium lamination, finally afterwards
Photoresist part and the layer gold being attached on photoetching offset plate figure or aluminium lamination are removed by stripping means, obtain required gold or aluminium
Interdigital electrode；
In the step 4, the gas-sensitive film layer of each subregion can use any suitable film growth techniques, generally
Different sensitive materials can be sprayed by mask baffle gas blowout method, is dried in vacuo after spraying, film-forming,
Prepare partition conbination resistance-type gas sensor.
When the different gas sensitives of each subregion of the present invention touch specific gas of the same race at the same time, every kind of material adsorbs gas to be measured
The change of response can be produced after body, swelling effect occurs or the electron hole based on electron hole exchange theory changes, each point
The response change of area's gas is superimposed to be caused to produce the comprehensive response to specific gas, so as to cause sensor to select gas
The raising of property.
In addition, gas sensitive material in test environment, due to being passed through the time restriction of carrier gas, inevitably exists
A degree of baseline drift, the sensitivity that the different baselines in carrier gas environment can be selected to drift about and drift about downwards upwards respectively
Material carries out error compensation, can compensate error caused by baseline drift so that the measurement accuracy of sensor has obtained significantly carrying
It is high.
Compared with the prior art, the invention has the advantages that：
1. the present invention has same specific gas in two symmetric partitionings coating using the center line of interdigital electrode as symmetry axis
There is the gas sensitive of different responses, gas sensitive combination of effects is obtained the comprehensive response of specific gas after being superimposed, improve to spy
Determine the selectivity of gas.
2. the present invention can to avoid traditional sensors composite sensitive film and multi-layer sensitive film desorption it is incomplete caused by base
Line drifting problem, the present invention are had the gas sensitive partition conbination of different responses using same specific gas, mutually compensated for, suppressed
The influence that baseline drift detects gas, improves the stability and measurement accuracy of gas sensor.
3. compared to composite membrane, multilayer film preparation process is complicated the shortcomings that, the present invention provide sensor construction it is simple, production
Cost is low, can be realized using traditional micro-processing technology.
4. resistance-type gas sensor structure provided by the invention, is different from the conventional method of composite membrane, multilayer film, for gas
The research of body sensor has started new approach with application.
Therefore, resistance-type gas sensor structure provided by the invention has boundless application prospect.
Brief description of the drawings
Fig. 1 is the structure diagram of one embodiment of the present of invention.
Fig. 2 is the structure and test schematic diagram of an example of the present invention.
Fig. 3 is single gas sensitive resistance-type gas sensor to NH3The resistance real-time response curve map of gas；Wherein,
(a) it is SnO2Gas sensitive resistance-type ammonia gas sensor is for various concentrations NH3Response curve, (b) for CuCl gas sensitives electricity
Resistive ammonia gas sensor is for various concentrations NH3Response curve, (c) is SnO2Gas sensitive resistance-type ammonia gas sensor for
Same concentrations NH3Repetition linearity curve, (d) for CuCl gas sensitive resistance-type ammonia gas sensors for same concentrations NH3Repetition
Linearity curve.
Fig. 4 is composite air-sensitive material resistance formula gas sensor to NH3The resistance real-time response curve map of gas；Wherein,
(e) for composite air-sensitive material resistance formula ammonia gas sensor for various concentrations NH3Response curve, (f) is composite air-sensitive material
Resistance-type ammonia gas sensor is for same concentrations NH3Repetition linearity curve.
Fig. 5 is the resistance-type ammonia gas sensor of the present invention to NH3The resistance real-time response curve map of gas；Wherein, (g) is
Resistance-type ammonia gas sensor of the present invention is for various concentrations NH3Response curve, (h) is resistance-type ammonia gas sensor pair of the present invention
In same concentrations NH3Repetition linearity curve.
Embodiment
The invention will be further described below in conjunction with the accompanying drawings：
As shown in Figure 1, a kind of resistance-type gas sensor, it is characterised in that including dielectric substrate, in dielectric substrate
Interdigital electrode and the gas-sensitive film layer that is deposited in interdigital electrode；The gas-sensitive film layer is with interdigital electrode
Symmetrical central axes are divided into two symmetrical region A and region B for symmetry axis in device surface, and region A sinks respectively with region B
Product has the gas-sensitive film layer for having different responses to same specific gas.
Embodiment：
The resistance-type ammonia gas sensor of the present invention is prepared, is comprised the following steps：
Step 1：It is substrate to select monocrystalline silicon, and substrate is cleaned and is pre-processed, by thermal oxidation method in substrate surface
Grow one layer of uniform silicon dioxide insulating layer；
Step 2：Photoresist is born with sol evenning machine spin coating on silica surface, using positive mask plate in deep UV lithography machine
Upper exposure, then development obtains mask graph in developer solution, is lithographically formed the golden interdigital electrode that 10 pairs of spacing are 50 μm and bears figure
Shape；
Step 3:The nickel chromium triangle for being 10nm with magnetron sputtering method sputtering thickness on the golden interdigital electrode negative patterning obtained by step 2
Alloy-layer, then layer gold of the vacuum vapour deposition evaporation thickness for 85nm is used in nickel chromium triangle layer surface, will finally by the method for stripping
Photoresist part and the layer gold being attached on photoetching offset plate figure remove, and obtain golden interdigital electrode；
Step 4：Two symmetrical subregions are formed in device surface using the symmetrical central axes of interdigital electrode as symmetry axis, are borrowed
Help the RGO and SnO that mask baffle is respectively 10wt% in a region spraying 0.5ml concentration with gas blowout method2Compound sensitive material
Material, in another region, spraying 0.5ml concentration is the RGO and CuCl of 10wt% compound sensitive material, by it after spraying
It is dried in vacuo, film-forming, resistance-type ammonia gas sensor of the present invention is made.
These three interdigital electrodes are made gas sensor and tested as a comparison by gas sensor needed for preparing contrast experiment's group
Demonstrate,prove the effect of the present invention.：
Make RGO and SnO that spraying 1ml concentration is 10wt%2Resistance-type gas of the composite solution as single gas sensitive
Body sensor, and spraying 1ml concentration sense for 10wt%RGO and resistance-type gas of the CuCl composite solutions as gas sensitization layer
Device,
Make the SnO of spraying 1ml2With resistance-type gas sensor of the CuCl composite solutions as composite air-sensitive material, institute
State RGO/SnO of the composite air-sensitive material by 1ml concentration for 10wt%2Solution is mixed with 1ml concentration for 10wt%RGO/CuCl solution
Close and prepare.
As shown in Fig. 2, above-mentioned four kinds of gas sensors are put into test box, be passed through nitrogen 8 it is small when after, each lead into concentration
For the NH of 20ppm, 40ppm, 60ppm, 80ppm, 100ppm3, the time is passed through every time as 15 minutes, and is being passed through various concentrations NH3
The pure nitrogen gas for being passed through 15 minutes again afterwards is recovered.
As shown in figure 3, using the single SnO of tradition2The resistance-type gas sensor of sensitive material and single CuCl are quick
The resistance-type gas sensor of material is felt to 0~100ppmNH3When being tested, SnO2Material sensors are under pure nitrogen gas environment
Initial resistance for 4500 Ω or so, be passed through the NH of 20~100ppm concentration in succession3When being passed through pure nitrogen gas again afterwards and being recovered,
The resistance of sensor can not return to initial resistance, overall that the obvious trend drifted about downwards is presented, to resistance when terminating to survey
Drop to 3870 Ω or so；Equally, the recovery resistance of resistance sensor made of single CuCl sensitive materials presents obvious
The trend drifted about upwards, while sensor made of both pure gas sensitive materials is to NH3Responsiveness it is smaller.
As shown in figure 4, two kinds of materials are directly mixed by the way of traditional, by SnO2The compound sensitivity with CuCl
Although resistance-type gas sensor prepared by material increases in responsiveness, but still have and be made with single CuCl materials
The identical baseline of resistance-type gas sensor seriously upper drift the problem of.
The sensor of structure of the present invention is employed as shown in figure 5, not only showing to NH3Larger responsiveness, Er Qie
Resistance can all return to initial resistance substantially during often wheel recovers, and the phenomenon of baseline drift has obtained good improvement, and
Good repeatability is shown in the repetitive test carried out under 60ppm.
In conclusion as shown in Fig. 3-Fig. 5：The resistance-type ammonia gas sensor of the present invention is to various concentrations NH3Selectivity
Improve, baseline drift phenomenon significantly reduces, and repeated experiment shows that stability is good, and overall each side is better than single gas sensitive
The gas sensor of gas sensor and composite air-sensitive material.
Described above is only presently preferred embodiments of the present invention, the present invention is not limited to enumerate above-described embodiment, should be said
Bright, any those skilled in the art are under the guidance of this specification, made equivalent substitute used, obvious change
Shape form, all falls within the essential scope of this specification, ought to be protected be subject to the present invention.
Claims (5)
- A kind of 1. resistance-type gas sensor, it is characterised in that interdigital electrode including dielectric substrate, in dielectric substrate with And it is deposited on the gas-sensitive film layer in interdigital electrode；The gas-sensitive film layer using the symmetrical central axes of interdigital electrode as Symmetry axis is divided into two symmetrical subregions in device surface, and each subregion has deposited respectively has same specific gas The gas-sensitive film layer of difference response.
- 2. resistance-type gas sensor according to claim 1, it is characterised in that the interdigital electrode material for gold or Aluminium.
- 3. resistance-type gas sensor according to claim 2, it is characterised in that the interdigital electrode logarithm is 10~15 It is right, refer to spacing as 10~100 μm.
- 4. a kind of preparation method of resistance-type gas sensor, it is characterised in that comprise the following steps：Step 1：Substrate is cleaned and is pre-processed, one layer of uniform titanium dioxide is grown in substrate surface by thermal oxidation method Silicon insulating layer；Step 2：Interdigital electrode logarithm is lithographically formed on silicon dioxide insulating layer as 10~15 pairs, refers to spacing as 10~100 μm Interdigital electrode negative patterning；Step 3:Sputtering forms nickel-chrome alloy layer on the interdigital electrode negative patterning obtained by step 2, then in nicr layer surface gold-plating Layer or aluminium lamination, finally remove unnecessary layer gold or aluminium lamination, obtain interdigital electrode；Step 4：Two symmetrical subregions are formed in device surface using the symmetrical central axes of interdigital electrode as symmetry axis, it is described each Subregion is the gas-sensitive film layer for having different responses to same specific gas, so that resistance-type gas sensor be made.
- 5. the preparation method of resistance-type gas sensor according to claim 4, it is characterised in that nickel in the step 3 The thickness of chromium alloy layer is 5~10nm, and the thickness of layer gold or aluminium lamination is 50~100nm.
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| CN106645308B (en) * | 2016-10-11 | 2020-09-29 | 南京工业大学 | Method for manufacturing acetone gas sensor based on alloy molybdenum disulfide tungsten nanosheets |
| CN108088876A (en) * | 2017-12-29 | 2018-05-29 | 扬州大学 | It is a kind of can thermometric air-sensitive film test device and its application method |
| CN113552295A (en) * | 2021-08-19 | 2021-10-26 | 电子科技大学 | Controllable growth lead sulfide composite film gas sensor and preparation method thereof |
| CN114047232A (en) * | 2021-11-25 | 2022-02-15 | 长春工业大学 | Preparation method of resistance type gas sensor based on sheet-shaped composite film |
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