CN106290482A - A kind of NO2the preparation method of Photo-electric gas-sensitivity sensor - Google Patents
A kind of NO2the preparation method of Photo-electric gas-sensitivity sensor Download PDFInfo
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- CN106290482A CN106290482A CN201610556969.6A CN201610556969A CN106290482A CN 106290482 A CN106290482 A CN 106290482A CN 201610556969 A CN201610556969 A CN 201610556969A CN 106290482 A CN106290482 A CN 106290482A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- 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
Abstract
The present invention relates to gas sensor preparing technical field, be specifically related to a kind of NO2The preparation method of Photo-electric gas-sensitivity sensor, the method comprises the following steps: prepared by step one, ZnO Seed Layer；Step 2, ZnO nano wall grow；Step 3, aging prepared finished product.NO prepared by the present invention2The advantage that Photo-electric gas-sensitivity sensor possesses following several respects: (1) may detect ppb level, the NO to 5ppb2Gas sensitivity be 7.482, (2) high sensitivity, is 6.16 to the luminous sensitivity that wavelength is 365nm light under room temperature, the NO to 50ppm2Sensitivity is up to 57.5, (3) good stability, and (4) material is easily obtained, and (5) have photosensitive and air-sensitive coupled characteristic.
Description
Technical field
The present invention relates to gas sensor preparing technical field, be specifically related to a kind of NO2The preparation of Photo-electric gas-sensitivity sensor
Method.
Background technology
Nitrogen dioxide is the gas of the irritant stink of a kind of brownish red, has severe corrosive and physiological stimulation effect, is
Form one of source of haze, be also one of the source of acid rain.Therefore, high selectivity, highly sensitive room temperature NO are studied2Gas
Sensor, to NO2Discharge carries out detecting accurately in real time, control and warning becomes too impatient to wait.
ZnO is a kind of important metal oxide semiconductor material, and energy gap is 3.37eV at normal temperatures, for directly band
Gap semiconductor, big to the absorptance of ultraviolet light, can sufficiently absorb ultraviolet light；And its carrier mobility is the highest, high
Electron mobility contribute to that there is bigger conductance and quick separation of charge；Its exciton bind energy is very big simultaneously, is about
60meV, has excellent photoelectric property.
In addition, the characteristic such as the dielectric unique and excellent due to it and piezoelectricity, it is widely used in gas sensor.Grind
Study carefully and show, ZnO when operating temperature is more than 200 DEG C to NO2There are preferable selectivity and higher sensitivity, detectable ppb
The NO of level2Gas.But, high operating temperature limits the gas sensor detection to flammable explosive gas, meanwhile, in high temperature work
Making in environment, metal-oxide crystal face can produce diffusion and sintering effect, thus affects sensor stability.Therefore, gas is reduced
The operating temperature of quick element, it is achieved at ambient temperature to NO2High selectivity, high sensitivity, become current ZnO sensor and grind
The major trend studied carefully.
So far, researcher is typically come by methods such as precious metal doping, transition metal oxide incorporation and light irradiations
Realize this target.Along with the fast development of LED technology, small-sized carrying ultraviolet, visible ray luminescence is achieved, light excites air-sensitive
Element Technology has obtained paying close attention to widely, and light irradiates before becoming and realizing the most valuable of high room temperature gas-sensitive property at present and have most
The method on way.
The layer of ZnO nanometer that utilized aqua-solution method and chemical vapour deposition technique at CdSe nano belt plated surface such as Bin Wu
Rod, forms ZnO/CdSe hetero-junctions, and it is under the conditions of optimum working temperature 160 DEG C, radiation of visible light, to 50ppm ethanol
Sensitivity is only 7.5.Yasin Sahin et al. utilizes hydro-thermal method to be prepared for zinc oxide nano rod on ito glass, and it is in work
When temperature is 30 DEG C, the sensitivity to white light is about 3.4, to 1ppm NO under the conditions of Halogen light irradiates2Sensitivity be only
1.316.Zheng Yang etc. utilizes hydro-thermal method to prepare CdS/ZnO core-shell structure copolymer hetero-junctions, and research shows this nucleocapsid structure
It is 0.68mW/cm at power2468nm light irradiate under, to 1ppm NO2The sensitivity of room temperature is 3.37.The profits such as Jiabao Cui
Being prepared for nanometer sheet, nano flower, the ZnO material of 3 kinds of different-shapes of nanofiber by method of electrostatic spinning and hydro-thermal method, it is in work
Under the conditions of temperature is room temperature, the irradiation of 365nm light, the sensitivity to 100ppm formaldehyde is respectively 1.88,4.95,12.61.By with
Upper report can show that light irradiates makes sensor be achieved at low-temperature working, but due to microstructures such as it is bar-shaped, lamellars
Impact, detecting concentration scope can only achieve ppm level.
Summary of the invention
It is an object of the invention to provide and there is under a kind of room temperature high sensitivity, the detectable NO to ppb level2Photo-electric gas-sensitivity passes
The preparation method of sensor, to overcome in prior art under room temperature condition NO2Sensitivity is low, the problem of detecting concentration narrow range.
For the problem overcoming prior art to exist, the technical solution that the present invention provides is: a kind of NO2Photo-electric gas-sensitivity
The preparation method of sensor, comprises the steps:
One, prepared by ZnO Seed Layer:
By the Zn (CH that mol ratio is 1:13COO)2·2H2O and Al (NO3)3.9H2O (Zinc diacetate dihydrate, analytical pure) and ethanol
Mix at ambient temperature, make Zn2+Concentration is 0.2mol/L, is placed in water-bath, heats with magnetic stirring apparatus and stir at 70 DEG C
Mix 1h, obtain uniform solution.After acetone, ethanol solution and deionized water ultrasonic cleaning 30min, and drying will be sequentially passed through
Ag interdigital electrode utilizes SYDC-100 Best-Effort request machine to lift, and pull rate is 4500 ~ 6000um/s, and dip time is
30s, is then dried 10min at 80 DEG C；Lifting 4 times repeatedly；The thin film heat treatment 30min at 400 DEG C that will obtain, obtains
ZnO seed tunic；
Two, ZnO nano wall growth:
By Zn (NO3)26H2O and (CH3)6N4The solution of 0.05mol/L it is configured in molar ratio for 1:1,70 DEG C of heated and stirred 1h,
After solution starting muddiness occurs, stop stirring, solution is poured in the polytetrafluoroethylliner liner of hydrothermal reaction kettle, and will cover
The Ag interdigital electrode having ZnO Seed Layer thin film is inserted perpendicularly in growth-promoting media, 80 DEG C of constant temperature growth 5h；Rush with deionized water after taking-up
Wash and be dried, obtain ZnO nano wall thin film, be finally putting in cabinet-type electric furnace heat treatment 1 h at 450 DEG C, in Ag interdigital electrode
Surface obtains one layer of white ZnO nano wall thin film；
Three, aging prepared finished product:
Ag interdigital electrode step 2 obtained is placed on CGS-1TP intelligence air-sensitive and analyzes system thermal station sample area, regulation two spy
Pin so that it is with two end in contact of electrode slice, during room temperature, at 365nm wavelength light (LED light source) illumination condition of irradiation power 100%
Under carry out aging, ageing time is 1.5h.
Beneficial effects of the present invention:
The NO provided2The gas sensitive of Photo-electric gas-sensitivity sensor is ZnO nano wall, and it is a kind of excellent two dimension sensing activity
Material, the network loose structure of three-dimensional communication so that it is have the advantages that volume is little, light weight, specific surface area are big；Big specific surface
The long-pending mechanical flexibility imparting material excellence, constructs again the passage that electronics, heat energy and load are effectively transmitted, for current-carrying simultaneously
Son transmission provides effective way；Meanwhile, ZnO is wide bandgap semiconductor materials, and its energy gap is 3.37 eV, to ultraviolet
The photoresponse of light is good.Therefore, porous ZnO nm wall photoelectric sensor has photosensitive and air-sensitive coupled characteristic, thus possesses
The advantage of several respects below: (1) may detect ppb level, the NO to 5ppb2Gas sensitivity be 7.482, (2) high sensitivity,
It is 6.16 to the luminous sensitivity that wavelength is 365nm light under room temperature, the NO to 50ppm2Sensitivity is up to 57.5, (3) good stability,
(4) material is easily obtained, and (5) have photosensitive and air-sensitive coupled characteristic.
Accompanying drawing explanation
Fig. 1 (a), (b) are that the ZnO nano wall of embodiment 1 preparation irradiates at the light that 365nm, irradiation power are 100% respectively
Under the conditions of to 50ppm, 5ppb NO2The air-sensitive of room temperature-photosensitive coupling response figure；C () is that the ZnO nano wall of embodiment 1 preparation exists
365nm, irradiation power be 100% light irradiate under the conditions of to 5ppb-5ppm NO2The air-sensitive of room temperature-photosensitive coupling response figure；
(d) be the ZnO nano wall of example 1 preparation be the photosensitive response figure of 100% to 365nm, irradiation power；E () is prepared by embodiment 1
ZnO nano wall in 365nm, different irradiation power illumination to 50ppm NO2The air-sensitive of room temperature-photosensitive coupling response figure；F () is
The ZnO nano wall of embodiment 1 preparation is at 365nm, the photosensitive response figure of different irradiation power illumination；G () is example 1 preparation
ZnO nano wall is 100% photosensitive response figure at a temperature of different operating to 365nm, irradiation power, to 50ppm NO2Room temperature
Air-sensitive-photosensitive coupling response figure；
Fig. 2 (a), (b) are that the ZnO nano wall of embodiment 2 preparation irradiates condition at the light that 365nm, irradiation power are 100% respectively
Under to 50ppm, 5ppb NO2The air-sensitive of room temperature-photosensitive coupling response figure；(c) be example 2 preparation ZnO nano wall to 365nm,
Irradiation power is the photosensitive response figure of 100%；
Fig. 3 (a), (b) are that the ZnO nano wall of embodiment 3 preparation irradiates condition at the light that 365nm, irradiation power are 100% respectively
Under to 50ppm, 5ppb NO2The air-sensitive of room temperature-photosensitive coupling response figure；(c) be example 3 preparation ZnO nano wall to 365nm,
Irradiation power is the photosensitive response figure of 100%；
Fig. 4 (a), (b) are that the ZnO nano wall of embodiment 4 preparation irradiates condition at the light that 365nm, irradiation power are 100% respectively
Under to 50ppm, 5ppb NO2The air-sensitive of room temperature-photosensitive coupling response figure；(c) be example 4 preparation ZnO nano wall to 365nm,
Irradiation power is the photosensitive response figure of 100%；
Fig. 5 is the XRD figure of the ZnO nano wall of embodiment 1 preparation；
Fig. 6 is the SEM figure of the ZnO nano wall of embodiment 1 preparation；
The TEM figure of the ZnO nano wall of Fig. 7 embodiment 1 preparation.
Detailed description of the invention
Below by embodiment and accompanying drawing, the present invention is described in detail:
Embodiment 1:
A kind of NO2The preparation method of Photo-electric gas-sensitivity sensor, comprises the steps:
1, prepared by Seed Layer
By the Zn (CH that mol ratio is 1:13COO)2·2H2O and Al (NO3)3.9H2O (Zinc diacetate dihydrate, analytical pure) and ethanol
Mix at ambient temperature, make Zn2+Concentration is 0.2mol/L, is placed in water-bath, heats with magnetic stirring apparatus and stir at 70 DEG C
Mix 1h, obtain uniform solution.Ag interdigital electrode sequentially passes through acetone, ethanol solution and deionized water ultrasonic cleaning (clean
Time is 30min), utilize SYDC-100 Best-Effort request machine to lift after drying, pull rate is 6000 μm/s, during dipping
Between be 30s, then at 80 DEG C be dried 10min；Lifting 4 times repeatedly；By thin film heat treatment 30min at 400 DEG C, obtain ZnO
Seed tunic.
2, ZnO nano wall growth
By Zn (NO3)26H2O and (CH3)6N4The solution of 0.05mol/L it is configured in molar ratio for 1:1,70 DEG C of heated and stirred 1h,
After solution starting muddiness occurs, stop stirring, solution is poured in the polytetrafluoroethylliner liner of hydrothermal reaction kettle, and will cover
The Ag interdigital electrode having ZnO Seed Layer thin film is inserted perpendicularly in growth-promoting media, 80 DEG C of constant temperature growth 5h；Rush with deionized water after taking-up
Wash and be dried, obtain ZnO nano wall thin film, be finally putting in cabinet-type electric furnace heat treatment 1 h at 450 DEG C, in Ag interdigital electrode
Surface obtains one layer of white ZnO nano wall thin film.
3, aging prepared finished product:
The Ag interdigital electrode sample that surface has been covered with ZnO nano wall thin film is placed on CGS-1TP intelligence air-sensitive analysis system temperature control
Platform sample area, regulates two probes so that it is with two end in contact of electrode slice.Temperature be room temperature, irradiation power be the 365nm ripple of 100%
Carrying out aging under light (LED light source) illumination condition of section, ageing time is 1.5h.
Performance detects:
The Photo-electric gas-sensitivity sensor obtaining the present embodiment carries out the detection of photosensitive property, through the resistance resistance of the sample of overaging
Value fluctuates within the specific limits, now cuts off light source, and resistance rises, and reopens light source after 50s, and resistance is replied, sensitive
Degree S is defined as: S=Rg/Ra(RaRepresent element resistance under illumination condition, RgRepresent resistance when element is cut off the electricity supply).ZnO
Nm wall to 365nm, irradiation power be 100% light irradiate under the conditions of to 5ppb-5ppm NO2The air-sensitive of room temperature-photosensitive coupling
Shown in response diagram such as Fig. 1 (c).ZnO nano wall to 365nm, irradiation power be 100% photosensitive response figure as shown in Figure 1 (d) shows；
ZnO nano wall in 365nm, different irradiation power illumination to 50ppm NO2The air-sensitive of room temperature-photosensitive coupling response figure such as Fig. 1
Shown in (e)；ZnO nano wall is shown at photosensitive response figure such as Fig. 1 (f) of 365nm, different irradiation power illumination；ZnO nano
Wall is 100% photosensitive response figure at a temperature of different operating to 365nm, irradiation power, to 50ppm NO2Air-sensitive-the light of room temperature
Shown in quick coupling response figure such as Fig. 1 (g)；
The Photo-electric gas-sensitivity sensor obtaining the present embodiment carries out the detection of photosensitive-air-sensitive coupling effect, through the sample of overaging
Resistance fluctuate within the specific limits, now inject NO2, cutting off light source simultaneously, resistance rises, and opens gas after 50s
Case, opens light source simultaneously, and resistance is replied, and sensitivity S is defined as S=Rg/Ra(RaRepresent that element has the resistance of illumination in atmosphere,
RgRepresent element resistance of unglazed photograph in tested gas).The ZnO nano wall of preparation is the light of 100% at 365nm, irradiation power
To 50ppm, 5ppb NO under the conditions of irradiation2Shown in the air-sensitive of room temperature-photosensitive coupling response figure such as Fig. 1 (a), (b).
Embodiment 2:
A kind of NO2The preparation method of Photo-electric gas-sensitivity sensor, comprises the steps:
1, prepared by Seed Layer
By the Zn (CH that mol ratio is 1:13COO)2·2H2O and Al (NO3)3.9H2O (Zinc diacetate dihydrate, analytical pure) and ethanol
Mix at ambient temperature, make Zn2+Concentration is 0.2mol/L, is placed in water-bath, heats with magnetic stirring apparatus and stir at 70 DEG C
Mix 1h, obtain uniform solution.Ag interdigital electrode sequentially passes through acetone, ethanol solution and deionized water ultrasonic cleaning (clean
Time is 30min), utilize SYDC-100 Best-Effort request machine to lift after drying, pull rate is 5500 μm/s, during dipping
Between be 30s, then at 80 DEG C be dried 10min；Lifting 4 times repeatedly；By thin film heat treatment 30min at 400 DEG C, obtain ZnO
Seed tunic.
2, ZnO nano wall growth
By Zn (NO3)26H2O and (CH3)6N4The solution of 0.05mol/L it is configured in molar ratio for 1:1,70 DEG C of heated and stirred 1h,
After solution starting muddiness occurs, stop stirring, solution is poured in the polytetrafluoroethylliner liner of hydrothermal reaction kettle, and will cover
The Ag interdigital electrode having ZnO Seed Layer thin film is inserted perpendicularly in growth-promoting media, 80 DEG C of constant temperature growth 5h；Rush with deionized water after taking-up
Wash and be dried, obtain ZnO nano wall thin film, be finally putting in cabinet-type electric furnace heat treatment 1 h at 450 DEG C, in Ag interdigital electrode
Surface obtains one layer of white ZnO nano wall thin film.
3, aging prepared finished product
The Ag interdigital electrode sample that surface has been covered with ZnO nano wall thin film is placed on CGS-1TP intelligence air-sensitive analysis system temperature control
Platform sample area, regulates two probes so that it is with two end in contact of electrode slice.Temperature be room temperature, irradiation power be the 365nm ripple of 100%
Carrying out aging under light (LED light source) illumination condition of section, ageing time is 1.5h.
Performance detects:
The Photo-electric gas-sensitivity sensor obtaining the present embodiment carries out the detection of photosensitive property, through the resistance of the sample of overaging
Fluctuating within the specific limits, now cut off light source, resistance rises, and reopens light source after 50s, and resistance is replied, sensitivity
S is defined as: S=Rg/Ra(RaRepresent element resistance under illumination condition, RgRepresent resistance when element is cut off the electricity supply).ZnO receives
Rice wall to 365nm, irradiation power be 100% photosensitive response figure such as Fig. 2 (c) shown.
The Photo-electric gas-sensitivity sensor obtaining the present embodiment carries out the detection of photosensitive-air-sensitive coupling effect, through overaging
The resistance of sample fluctuates within the specific limits, now injects NO2, cutting off light source simultaneously, resistance rises, and takes off after 50s
Driving gas tank, open light source simultaneously, resistance is replied, and sensitivity S is defined as S=Rg/Ra(RaRepresent that element has the electricity of illumination in atmosphere
Resistance, RgRepresent element resistance of unglazed photograph in tested gas).The ZnO nano wall of preparation is 100% at 365nm, irradiation power
Light light irradiate under the conditions of to 50ppm, 5ppb NO2Shown in the air-sensitive of room temperature-photosensitive coupling response figure such as Fig. 2 (a), (b).
Embodiment 3:
A kind of NO2The preparation method of Photo-electric gas-sensitivity sensor, comprises the steps:
1, prepared by Seed Layer
By the Zn (CH that mol ratio is 1:13COO)2·2H2O and Al (NO3)3.9H2O (Zinc diacetate dihydrate, analytical pure) and ethanol
Mix at ambient temperature, make Zn2+Concentration is 0.2mol/L, is placed in water-bath, heats with magnetic stirring apparatus and stir at 70 DEG C
Mix 1h, obtain uniform solution.Ag interdigital electrode sequentially passes through acetone, ethanol solution and deionized water ultrasonic cleaning (clean
Time is 30min), utilize SYDC-100 Best-Effort request machine to lift after drying, pull rate is 5000 μm/s, during dipping
Between be 30s, then at 80 DEG C be dried 10min；Lifting 4 times repeatedly；By thin film heat treatment 30min at 400 DEG C, obtain ZnO
Seed tunic.
2, ZnO nano wall growth
By Zn (NO3)26H2O and (CH3)6N4The solution of 0.05mol/L it is configured in molar ratio for 1:1,70 DEG C of heated and stirred 1h,
After solution starting muddiness occurs, stop stirring, solution is poured in the polytetrafluoroethylliner liner of hydrothermal reaction kettle, and will cover
The Ag interdigital electrode having ZnO Seed Layer thin film is inserted perpendicularly in growth-promoting media, 80 DEG C of constant temperature growth 5h；Rush with deionized water after taking-up
Wash and be dried, obtain ZnO nano wall thin film, be finally putting in cabinet-type electric furnace heat treatment 1 h at 450 DEG C, in Ag interdigital electrode
Surface obtains one layer of white ZnO nano wall thin film.
3, aging prepared finished product
The Ag interdigital electrode sample that surface has been covered with ZnO nano wall thin film is placed on CGS-1TP intelligence air-sensitive analysis system temperature control
Platform sample area, regulates two probes so that it is with two end in contact of electrode slice.Temperature be room temperature, irradiation power be the 365nm ripple of 100%
Carrying out aging under light (LED light source) illumination condition of section, ageing time is 1.5h.
Performance detects:
The Photo-electric gas-sensitivity sensor obtaining the present embodiment carries out the detection of photosensitive property, through the resistance of the sample of overaging
Fluctuating within the specific limits, now cut off light source, resistance rises, and reopens light source after 50s, and resistance is replied, sensitivity
S is defined as: S=Rg/Ra(RaRepresent element resistance under illumination condition, RgRepresent resistance when element is cut off the electricity supply).ZnO receives
Rice wall to 365nm, irradiation power be 100% photosensitive response figure such as Fig. 3 (c) shown.
The Photo-electric gas-sensitivity sensor obtaining the present embodiment carries out the detection of photosensitive-air-sensitive coupling effect, through overaging
The resistance of sample fluctuates within the specific limits, now injects NO2, cutting off light source simultaneously, resistance rises, and takes off after 50s
Driving gas tank, open light source simultaneously, resistance is replied, and sensitivity S is defined as S=Rg/Ra(RaRepresent that element has the electricity of illumination in atmosphere
Resistance, RgRepresent element resistance of unglazed photograph in tested gas).The ZnO nano wall of preparation is 100% at 365nm, irradiation power
Light irradiate under the conditions of to 50ppm, 5ppb NO2Shown in the air-sensitive of room temperature-photosensitive coupling response figure such as Fig. 3 (a), (b).
Embodiment 4:
A kind of NO2The preparation method of Photo-electric gas-sensitivity sensor, comprises the steps:
1, prepared by Seed Layer
By the Zn (CH that mol ratio is 1:13COO)2·2H2O and Al (NO3)3.9H2O (Zinc diacetate dihydrate, analytical pure) and ethanol
Mix at ambient temperature, make Zn2+Concentration is 0.2mol/L, is placed in water-bath, heats with magnetic stirring apparatus and stir at 70 DEG C
Mix 1h, obtain uniform solution.Ag interdigital electrode sequentially passes through acetone, ethanol solution and deionized water ultrasonic cleaning (clean
Time is 30min), utilize SYDC-100 Best-Effort request machine to lift after drying, pull rate is 4500 μm/s, during dipping
Between be 30s, then at 80 DEG C be dried 10min；Lifting 4 times repeatedly；By thin film heat treatment 30min at 400 DEG C, obtain ZnO
Seed tunic.
2, ZnO nano wall growth
By Zn (NO3)26H2O and (CH3)6N4The solution of 0.05mol/L it is configured in molar ratio for 1:1,70 DEG C of heated and stirred 1h,
After solution starting muddiness occurs, stop stirring, solution is poured in the polytetrafluoroethylliner liner of hydrothermal reaction kettle, and will cover
The Ag interdigital electrode having ZnO Seed Layer thin film is inserted perpendicularly in growth-promoting media, 80 DEG C of constant temperature growth 5h；Rush with deionized water after taking-up
Wash and be dried, obtain ZnO nano wall thin film, be finally putting in cabinet-type electric furnace heat treatment 1 h at 450 DEG C, in Ag interdigital electrode
Surface obtains one layer of white ZnO nano wall thin film.
3, aging prepared finished product
The Ag interdigital electrode sample that surface has been covered with ZnO nano wall thin film is placed on CGS-1TP intelligence air-sensitive analysis system temperature control
Platform sample area, regulates two probes so that it is with two end in contact of electrode slice.Temperature be room temperature, irradiation power be the 365nm ripple of 100%
Carrying out aging under light (LED light source) illumination condition of section, ageing time is 1.5h.
Performance detects:
The Photo-electric gas-sensitivity sensor obtaining the present embodiment carries out the detection of photosensitive property, through the resistance of the sample of overaging
Fluctuating within the specific limits, now cut off light source, resistance rises, and reopens light source after 50s, and resistance is replied, sensitivity
S is defined as: S=Rg/Ra(RaRepresent element resistance under illumination condition, RgRepresent resistance when element is cut off the electricity supply).ZnO receives
Rice wall to 365nm, irradiation power be 100% photosensitive response figure such as Fig. 4 (c) shown.
The Photo-electric gas-sensitivity sensor obtaining the present embodiment carries out the detection of photosensitive-air-sensitive coupling effect, through overaging
The resistance of sample fluctuates within the specific limits, now injects NO2, cutting off light source simultaneously, resistance rises, and takes off after 50s
Driving gas tank, open light source simultaneously, resistance is replied, and sensitivity S is defined as S=Rg/Ra(RaRepresent that element has the electricity of illumination in atmosphere
Resistance, RgRepresent element resistance of unglazed photograph in tested gas).The ZnO nano wall of preparation is 100% at 365nm, irradiation power
Light irradiate under the conditions of to 50ppm, 5ppb NO2Shown in the air-sensitive of room temperature-photosensitive coupling response figure such as Fig. 4 (a), (b).
The Photo-electric gas-sensitivity sensor obtained with embodiment 1, carries out related experiment, and result is as follows:
The XRD figure of (a) ZnO nano wall
Seeing Fig. 5, ZnO nano wall is along [002] direction preferential growth, and has higher crystalline quality.
The SEM figure of (b) ZnO nano wall
See Fig. 6, there is the ZnO nano wall of loose structure, along the orientation periodic arrangement growth of Ag interdigital electrode vertical direction.
Photosensitive and the air-sensitive of (c) ZnO nano wall-photosensitive coupling effect figure
See Fig. 1 understand, under the conditions of the sensor room temperature prepared by embodiment 1 under to the sensitivity that wavelength is 365nm light be
6.16, the NO to 5ppb2Sensitivity is 7.482, the NO to 50ppm2Sensitivity is 57.5, is significantly larger than other documents report
Sensitivity.In addition, by the research to operating temperature, it can be deduced that along with the rising of operating temperature, its sensitive to light
Degree reduces, and the sensitivity to detected gas also decreases.By the research to illumination power, draw the reduction along with power,
The sensitivity of light is reduced by it, and the sensitivity to detected gas reduces the most therewith.
Present disclosure is not limited to cited by embodiment, and those of ordinary skill in the art are by reading description of the invention
And the conversion of any equivalence that technical solution of the present invention is taked, the claim being the present invention is contained.
Claims (1)
1. a NO2The preparation method of Photo-electric gas-sensitivity sensor, it is characterised in that: comprise the steps:
Prepared by step one, ZnO Seed Layer:
By the Zn (CH that mol ratio is 1:13COO)2·2H2O and Al (NO3)3.9H2O mixes at ambient temperature with ethanol, makes Zn2 +Concentration is 0.2mol/L, is placed in water-bath, by magnetic stirring apparatus heated and stirred 1h at 70 DEG C, obtains uniform solution；Will
Ag interdigital electrode sequentially passes through acetone, ethanol solution and deionized water ultrasonic cleaning 30min, utilizes SYDC-100 to impregnate after drying
Pulling machine lifts, and pull rate is 4500 ~ 6000um/s, and dip time is 30s, is then dried 10min at 80 DEG C；Instead
Lifting 4 times again；The thin film heat treatment 30min at 400 DEG C that will generate, obtains ZnO seed tunic；
Step 2, ZnO nano wall grow:
By Zn (NO3)26H2O and (CH3)6N4The solution of 0.05mol/L it is configured in molar ratio for 1:1,70 DEG C of heated and stirred 1h,
After solution starting muddiness occurs, stop stirring, solution is poured in the polytetrafluoroethylliner liner of hydrothermal reaction kettle, and will cover
The Ag interdigital electrode having ZnO Seed Layer thin film is inserted perpendicularly in growth-promoting media, 80 DEG C of constant temperature growth 5h；Rush with deionized water after taking-up
Wash and be dried, obtain ZnO nano wall thin film, be finally putting in cabinet-type electric furnace heat treatment 1 h at 450 DEG C, i.e. at the interdigital electricity of Ag
Surface, pole obtains one layer of white ZnO nano wall thin film；
Step 3, aging prepared finished product:
Ag interdigital electrode step 2 obtained is placed on CGS-1TP intelligence air-sensitive and analyzes system thermal station sample area, regulation two spy
Pin so that it is with two end in contact of electrode slice, during room temperature, carry out old under the 365nm wavelength light illumination condition of irradiation power 100%
Changing, ageing time is 1.5h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109030578A (en) * | 2018-07-30 | 2018-12-18 | 清华大学 | A kind of NO based on the nano heterogeneous junction structure of CdTe/ZnO2The preparation method of gas sensor |
| CN110498440A (en) * | 2019-07-11 | 2019-11-26 | 江苏大学 | A kind of zinc oxide air-sensitive membrane material, preparation method and applications |
| CN114993972A (en) * | 2022-05-27 | 2022-09-02 | 江南大学 | ZnO nanowire and NO 2 Gas sensor, its preparation and application |
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| CN103628133A (en) * | 2013-12-09 | 2014-03-12 | 西安工业大学 | Method for preparing aqueous solution of directional growth monocrystalline ZnO nano wall |
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| CN103628133A (en) * | 2013-12-09 | 2014-03-12 | 西安工业大学 | Method for preparing aqueous solution of directional growth monocrystalline ZnO nano wall |
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| CN109030578A (en) * | 2018-07-30 | 2018-12-18 | 清华大学 | A kind of NO based on the nano heterogeneous junction structure of CdTe/ZnO2The preparation method of gas sensor |
| CN110498440A (en) * | 2019-07-11 | 2019-11-26 | 江苏大学 | A kind of zinc oxide air-sensitive membrane material, preparation method and applications |
| CN114993972A (en) * | 2022-05-27 | 2022-09-02 | 江南大学 | ZnO nanowire and NO 2 Gas sensor, its preparation and application |
| CN114993972B (en) * | 2022-05-27 | 2023-08-11 | 江南大学 | ZnO nanowire and NO 2 Gas sensor, its preparation and application |
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