CN103344568A - Method for photoelectrically detecting nitrogen dioxide with trace amount - Google Patents

Method for photoelectrically detecting nitrogen dioxide with trace amount Download PDF

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Publication number
CN103344568A
CN103344568A CN2013103012129A CN201310301212A CN103344568A CN 103344568 A CN103344568 A CN 103344568A CN 2013103012129 A CN2013103012129 A CN 2013103012129A CN 201310301212 A CN201310301212 A CN 201310301212A CN 103344568 A CN103344568 A CN 103344568A
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sensitive material
light source
sensor
light
resistance
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祖佰祎
窦新存
陆彬
郭亚楠
杨政
郭林娟
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Abstract

The invention relates to a method for photoelectrically detecting nitrogen dioxide with trace amount. A resistive sensor comprises a ceramic substrate, a fixed electrode, a sensitive material, a heater, a thermocouple, a signal processor and a light source. By utilizing the photoconductive effect of the sensitive material of the resistive sensor, light with a 200-800nm wavelength range is irradiated onto the sensitive material, and the nitrogen dioxide with the trace amount is detected through the change in resistance of the sensitive material, so that the NO2 detection limit is improved and simultaneously the working temperature is reduced. The method not only can improve the detection limit (reach ppb level), but also reduces the working temperature (room temperature to 220 DEG C).

Description

A kind of method of Photoelectric Detection trace nitrogen dioxide
Technical field
The present invention relates to a kind of trace NO 2Photoelectric detecting method.Be specifically related to use the illumination of certain wavelength coverage to penetrate resistance-type NO 2The sensitive material of gas sensor is by adsorbed NO 2The semi-conductive photoconduction that gas causes changes, to trace NO 2Detect and demarcate.This method can improve detectability (reach the ppb level, namely part per billion, reduce working temperature (room temperature to 220 ℃) in the time of V/V).
Background technology
At present, NO 2Resistance sensor utilize gas when semiconductor (mostly being metal oxide) surface absorption or desorption, the semiconductor resistor variation detects, exist working temperature height (300 ℃-850 ℃) (Sensors and Actuators B 158,2011,1 – 8) and low (the ppm level of detectability, namely 1,000,000/, shortcoming V/V).
When incident photon energy (
Figure 203782DEST_PATH_IMAGE001
) more than or equal to semi-conductive energy gap (E g) time, the electronics in the valence band can absorb incident photon, transits to conduction band by valence band, produces photo-generated carrier, causes that conductivity semiconductor changes, and is called photoconductive effect.The condition that produces photoconductive effect is that the incident light energy is greater than this semi-conductive energy gap.
The present invention utilizes the photoconductive effect of sensitive material, uses photoelectric method to detect NO 2, reach the purpose that reduces working temperature when improving detectability.
Summary of the invention
The object of the present invention is to provide a kind of method of Photoelectric Detection trace nitrogen dioxide, the resistance sensor that this method relates to is made up of ceramic bases, fixed electorde, sensitive material, well heater and thermopair, signal processor and light source, utilize the photoconductive effect of the sensitive material of resistance sensor, use the illumination of 200-800 nm wavelength coverage to penetrate sensitive material, resistance variations by sensitive material detects trace nitrogen dioxide, realizes improving NO 2Reduce working temperature in the time of detectability.This method not only can improve detectability (reaching the ppb level), can reduce simultaneously working temperature (room temperature to 220 ℃).
The method of a kind of Photoelectric Detection trace nitrogen dioxide of the present invention, the resistance sensor that this method relates to is made up of ceramic bases (1), fixed electorde (2), sensitive material (3), well heater and thermopair (4), signal processor (5) and light source (6), utilize the photoconductive effect of the sensitive material of resistance sensor, use the illumination of 200-800 nm wavelength coverage to penetrate sensitive material (3), resistance variations by sensitive material (3) detects trace nitrogen dioxide, and concrete operations follow these steps to carry out:
A, go up fixed electorde (2) in ceramic bases (1), by sensitive material (3) electrode (2) is communicated with, electrode (2) is connected with signal processor (5), and well heater and thermopair (4) are fixed on the bottom of ceramic bases (1), constitutes resistance sensor;
B, with light source (6) wavelength coverage above the light emitting diode between the 200-800 nm, Xe lamp, Hg lamp or LASER Light Source are fixed on the sensor that step a makes, sensor is placed the NO that contains concentration known 2In the atmosphere, in room temperature to 500 ℃, at light source (6) 0-100 W/m 2Under the light intensity condition, irradiation sensitive material (3) is signal with the resistance variations of sensitive material (3), and sensor is demarcated;
C, sensor placed the NO that contains unknown concentration 2Atmosphere in, in room temperature to 500 ℃, at light source (6) 0-100 W/m 2Under the light intensity condition, to trace NO 2Carry out Photoelectric Detection.
Be single component semiconductor material nickel oxide, molybdena, cuprous oxide, tungstic acid, tin ash, zinc paste or carbon nano-tube in the step a sensitive material (3); The heterojunction semiconductor material is tin ash/zinc paste; Composite semiconductor material is yttria-stabilized zirconia or titania/Graphene.
The wavelength coverage of step b light source (6) is between 200-800 nm, and light source (6) photon energy is more than or equal to the energy gap of the less semiconductor material of heterojunction semiconductor material in the sensitive material (3) or composite semiconductor material energy gap.
Light source (6) uses grating, filter plate, lens and catoptron that light is treated to monochromatic light when sending polychromatic light among step b and the step c.
Light source among the step b (6) is light emitting diode.
The method of a kind of Photoelectric Detection trace nitrogen dioxide of the present invention adopts this method can make detectability be increased to 1 ppb, and simultaneously, working temperature reduces about 100 ℃.
Description of drawings
Fig. 1 is the structural representation of sensor of the present invention;
Fig. 2 is the ultraviolet-visible absorbance figure of sensitive material titania/graphene composite material of the present invention;
Fig. 3 for the present invention with titania/graphene composite material be sensitive material under 220 ℃ of conditions of temperature to variable concentrations NO 2Response curve: 100 ppb, 200 ppb, 500 ppb, 1000 ppb;
Fig. 4 for the present invention with titania/graphene composite material be sensitive material under 220 ℃ of conditions of temperature to NO 2The calibration curve of Photoelectric Detection;
Fig. 5 is sensitive material dark condition and optical condition detection NO under 100 ℃ of conditions of temperature for the present invention with titania/graphene composite material 2Performance comparison figure, wherein-█-expression optical condition under corresponding to NO 2Concentration is respectively the responsiveness of 1.25 ppb, 2.5 ppb, 5 ppb, 10 ppb, 20 ppb, 50 ppb, 100 ppb and 200 ppb;-●-represent under the dark condition corresponding to NO 2Concentration is respectively the responsiveness of 10 ppb, 20 ppb, 50 ppb, 100 ppb, 200 ppb;
Fig. 6 for the present invention with titania/graphene composite material be sensitive material under 220 ℃ of conditions of temperature to 500 ppb NO 2The response time figure of Photoelectric Detection.
Embodiment:
Below in conjunction with drawings and Examples this patent is elaborated:
Embodiment 1
The making of resistance sensor:
Fixed electorde 2 on ceramic bases 1, by sensitive material titania/Graphene 3 electrode 2 are communicated with, and electrode 2 is connected with signal processor 5, and well heater and thermopair 4 are fixed on the bottom of ceramic bases 1, constitute resistance sensor;
Photoelectric Detection NO 2Method:
Increasing wavelength directly over resistance sensor is light emitting diode (LED) light source 6 of 367 nm, as shown in Figure 1, sensor is placed the NO that contains concentration known 2In the atmosphere, be 9 W/m in 220 ℃ of temperature and light source 6 2Under the light intensity condition, irradiation sensitive material titania/graphene composite material 3 is signal with titania/graphene composite material 3 resistance variations, and sensor is demarcated;
Again sensor is placed the NO that contains unknown concentration 2Atmosphere in, be 9 W/m in 220 ℃ of temperature and light source 6 2Under the light intensity condition, to trace NO 2Carry out Photoelectric Detection.
Embodiment 2
The making of resistance sensor is carried out according to embodiment 1;
Photoelectric Detection NO 2Method:
Increase Xe lamp source 6 in the oblique upper of resistance sensor, use grating, filter plate, lens and catoptron that light is treated to monochromatic light, making wavelength is that the illumination of 200 nm is penetrated in sensitive material titania/graphene composite material 3; The absorption of 3 pairs of different wavelengths of light of titania/graphene composite material places sensor the NO that contains concentration known as shown in Figure 2 2In the atmosphere, be 0.001 W/m in room temperature and light source 6 2Under the light intensity condition, be signal with the resistance variations of sensitive material titania/graphene composite material 3, sensor is demarcated;
Again sensor is placed the NO that contains unknown concentration 2Atmosphere in, be 0.001 W/m in room temperature and light source 6 2Under the light intensity condition, to trace NO 2Carry out Photoelectric Detection.
Embodiment 3
The making of resistance sensor:
Fixed electorde 2 on ceramic bases 1, by sensitive material nickel oxide 3 electrode 2 are communicated with, and electrode 2 is connected with signal processor 5, and well heater and thermopair 4 are fixed on the bottom of ceramic bases 1, constitute resistance sensor;
Photoelectric Detection NO 2Method:
Directly over resistance sensor, increase Xe lamp source 6, as shown in Figure 1, sensor is placed the NO that contains concentration known 2In the atmosphere, being signal with the resistance variations of sensitive material nickel oxide material 3, is 0.001 W/m in 100 ℃ of temperature and light source 6 2Under the light intensity condition, sensor is demarcated;
Again sensor is placed the NO that contains unknown concentration 2Atmosphere in, be 0.001 W/m in 100 ℃ of temperature and light source 6 2Under the light intensity condition, to trace NO 2Carry out Photoelectric Detection.
Embodiment 4
The making of resistance sensor:
Fixed electorde 2 on ceramic bases 1, by sensitive material molybdena 3 electrode 2 are communicated with, and electrode 2 is connected with signal processor 5, and well heater and thermopair 4 are fixed on the bottom of ceramic bases 1, constitute resistance sensor;
Photoelectric Detection NO 2Method:
Increasing wavelength directly over resistance sensor is the Hg lamp source 6 of 800 nm, as shown in Figure 1, sensor is placed the NO that contains concentration known 2In the atmosphere, being signal with sensitive material molybdena 3 resistance variations, is 100 W/m in room temperature and light source 6 2Under the light intensity condition, sensor is demarcated;
Again sensor is placed the NO that contains unknown concentration 2Atmosphere in, be 100 W/m in room temperature and light source 6 2Under the light intensity condition, to trace NO 2Carry out Photoelectric Detection.
Embodiment 5
The making of resistance sensor:
Fixed electorde 2 on ceramic bases 1, by sensitive material cuprous oxide 3 electrode 2 are communicated with, and electrode 2 is connected with signal processor 5, and well heater and thermopair 4 are fixed on the bottom of ceramic bases 1, constitute resistance sensor;
Photoelectric Detection NO 2Method:
Increasing wavelength directly over resistance sensor is the LASER Light Source 6 of 405 nm, as shown in Figure 1, sensor is placed the NO that contains concentration known 2In the atmosphere, being signal with sensitive material cuprous oxide 3 resistance variations, is 10 W/m in room temperature and light source 6 2Under the light intensity condition, sensor is demarcated;
Again sensor is placed the NO that contains unknown concentration 2Atmosphere in, be 10 W/m in room temperature and light source 6 2Under the light intensity condition, to trace NO 2Carry out Photoelectric Detection.
Embodiment 6
The making of resistance sensor:
Fixed electorde 2 on ceramic bases 1, by sensitive material tungstic acid 3 electrode 2 are communicated with, and electrode 2 is connected with signal processor 5, and well heater and thermopair 4 are fixed on the bottom of ceramic bases 1, constitute resistance sensor;
Photoelectric Detection NO 2Method:
Increasing wavelength directly over resistance sensor is light emitting diode (LED) light source 6 of 250 nm, as shown in Figure 1, sensor is placed the NO that contains concentration known 2In the atmosphere, being signal with sensitive material tungstic acid 3 resistance variations, is 10 W/m in room temperature and light source 6 2Under the light intensity condition, sensor is demarcated;
Again sensor is placed the NO that contains unknown concentration 2Atmosphere in, be 10 W/m in room temperature and light source 6 2Under the light intensity condition, to trace NO 2Carry out Photoelectric Detection.
Embodiment 7
The making of resistance sensor:
Fixed electorde 2 on ceramic bases 1, by sensitive material tin ash 3 electrode 2 are communicated with, and electrode 2 is connected with signal processor 5, and well heater and thermopair 4 are fixed on the bottom of ceramic bases 1, constitute resistance sensor;
Photoelectric Detection NO 2Method:
Increasing wavelength directly over resistance sensor is light emitting diode (LED) light source 6 of 300 nm, as shown in Figure 1, sensor is placed the NO that contains concentration known 2In the atmosphere, being signal with sensitive material tin ash 3 resistance variations, is 10 W/m in 500 ℃ of temperature and light source 6 2Under the light intensity condition, sensor is demarcated;
Again sensor is placed the NO that contains unknown concentration 2Atmosphere in, be 10 W/m in 500 ℃ of temperature and light source 6 2Under the light intensity condition, to trace NO 2Carry out Photoelectric Detection.
Embodiment 8
The making of resistance sensor:
Fixed electorde 2 on ceramic bases 1, by sensitive material zinc paste 3 electrode 2 are communicated with, and electrode 2 is connected with signal processor 5, and well heater and thermopair 4 are fixed on the bottom of ceramic bases 1, constitute resistance sensor;
Photoelectric Detection NO 2Method:
Increasing wavelength directly over resistance sensor is light emitting diode (LED) light source 6 of 350 nm, as shown in Figure 1, sensor is placed the NO that contains concentration known 2In the atmosphere, being signal with sensitive material zinc paste 3 resistance variations, is 1 W/m in 100 ℃ of temperature and light source 6 2Under the light intensity condition, sensor is demarcated;
Again sensor is placed the NO that contains unknown concentration 2Atmosphere in, be 1 W/m in 100 ℃ of temperature and light source 6 2Under the light intensity condition, to trace NO 2Carry out Photoelectric Detection.
Embodiment 9
The making of resistance sensor:
Fixed electorde 2 on ceramic bases 1, by sensitive material carbon nano-tube 3 electrode 2 are communicated with, and electrode 2 is connected with signal processor 5, and well heater and thermopair 4 are fixed on the bottom of ceramic bases 1, constitute resistance sensor;
Photoelectric Detection NO 2Method:
Increasing wavelength directly over resistance sensor is light emitting diode (LED) light source 6 of 400 nm, as shown in Figure 1, sensor is placed the NO that contains concentration known 2In the atmosphere, being signal with sensitive material carbon nano-tube 3 resistance variations, is 8 W/m in 100 ℃ of temperature and light source 6 2Under the light intensity condition, sensor is demarcated;
Again sensor is placed the NO that contains unknown concentration 2Atmosphere in, be 8 W/m in 100 ℃ of temperature and light source 6 2Under the light intensity condition, to trace NO 2Carry out Photoelectric Detection.
Embodiment 10
The making of resistance sensor:
Fixed electorde 2 on ceramic bases 1, by sensitive material tin ash/zinc oxide heterogeneous knot material 3 electrode 2 are communicated with, and electrode 2 is connected with signal processor 5, and well heater and thermopair 4 are fixed on the bottom of ceramic bases 1, constitute resistance sensor;
Photoelectric Detection NO 2Method:
Increasing wavelength directly over resistance sensor is light emitting diode (LED) light source 6 of 450 nm, as shown in Figure 1, sensor is placed the NO that contains concentration known 2In the atmosphere, being signal with sensitive material tin ash/zinc oxide material 3 resistance variations, is 1 W/m in 400 ℃ of temperature and light source 6 2Under the light intensity condition, sensor is demarcated;
Again sensor is placed the NO that contains unknown concentration 2Atmosphere in, be 1 W/m in 400 ℃ of temperature and light source 6 2Under the light intensity condition, to trace NO 2Carry out Photoelectric Detection.
Embodiment 11
The making of resistance sensor:
Fixed electorde 2 on ceramic bases 1, by sensitive material yttria-stabilized zirconia compound substance 3 electrode 2 are communicated with, and electrode 2 is connected with signal processor 5, and well heater and thermopair 4 are fixed on the bottom of ceramic bases 1, constitute resistance sensor;
Photoelectric Detection NO 2Method:
Increasing wavelength directly over resistance sensor is light emitting diode (LED) light source 6 of 500 nm, as shown in Figure 1, sensor is placed the NO that contains concentration known 2In the atmosphere, being signal with sensitive material yttria-stabilized zirconia compound substance 3 resistance variations, is 8 W/m in 500 ℃ of temperature and light source 6 2Under the light intensity condition, sensor is demarcated;
Again sensor is placed the NO that contains unknown concentration 2Atmosphere in, be 8 W/m in 500 ℃ of temperature and light source 6 2Under the light intensity condition, to trace NO 2Carry out Photoelectric Detection.
Embodiment 12
The making of resistance sensor is carried out according to embodiment 1;
Photoelectric Detection NO 2Method:
Increase Hg lamp source 6 directly over sensor, using the monochromator output wavelength is that the illumination of 400 nm is penetrated in sensitive material titania/Graphene composite wood 3 resistance variations and is signal, is 9 W/m in 200 ℃ of temperature of temperature and light source 6 2Under the light intensity condition, carry out transducer calibration;
Again sensor is placed the NO that contains unknown concentration 2Atmosphere in, be 9 W/m in 200 ℃ of temperature and light source 6 2Under the light intensity condition, to trace NO 2Carry out Photoelectric Detection.
Embodiment 13
The making of resistance sensor and Photoelectric Detection NO 2Method carry out according to embodiment 1;
Under 220 ℃ of the temperature to variable concentrations NO 2Response results as shown in Figure 3, NO 2In material surface absorption, its resistance reduces, and corresponding response concentration is 100 ppb, 200 ppb, 500 ppb, 1000 ppb; Its calibration result as shown in Figure 4, fit equation is the Langmuir equation at constant temperature
Figure 538949DEST_PATH_IMAGE002
, wherein
Figure 80920DEST_PATH_IMAGE003
Be responsiveness, the number percent of resistance value in the difference of resistance value (Ra) and the air is (Rg-Ra)/Ra * 100% in the resistance value when being defined as adsorbed gas (Rg) and the air, and C is NO 2Concentration, A=94.16, B=-4550.47.
Embodiment 14
The making of resistance sensor is carried out according to embodiment 1;
Under 100 ℃ of the temperature, be that the led light source of 367 nm is at 9 W/m at dark condition and wavelength respectively 2Light intensity irradiation down to NO 2The detection performance comparison as shown in Figure 5, under-█-expression optical condition corresponding to NO 2Concentration is respectively the responsiveness of 1.25 ppb, 2.5 ppb, 5 ppb, 10 ppb, 20 ppb, 50 ppb, 100 ppb and 200 ppb;-●-represent under the dark condition corresponding to NO 2Concentration is respectively the responsiveness of 10 ppb, 20 ppb, 50 ppb, 100 ppb, 200 ppb; The method of Photoelectric Detection can make NO 2Detectability improves about 1 order of magnitude.
Embodiment 15
The making of resistance sensor is carried out according to embodiment 1;
Under 200 ℃ of conditions of temperature, to the NO of 500 ppb 2The response time of gas and release time are defined as response time and release time resistance change respectively and are 90% used time of total variation, NO as shown in Figure 6 2In material surface absorption, its resistance reduces, and the response time is 133 s; NO 2From the material surface desorption, its resistance increases, and be 100 s release time.

Claims (5)

1. the method for a Photoelectric Detection trace nitrogen dioxide, it is characterized in that the resistance sensor that this method relates to is made up of ceramic bases (1), fixed electorde (2), sensitive material (3), well heater and thermopair (4), signal processor (5) and light source (6), utilize the photoconductive effect of the sensitive material of resistance sensor, use the illumination of 200-800 nm wavelength coverage to penetrate sensitive material (3), resistance variations by sensitive material (3) detects trace nitrogen dioxide, and concrete operations follow these steps to carry out:
A, go up fixed electorde (2) in ceramic bases (1), by sensitive material (3) electrode (2) is communicated with, electrode (2) is connected with signal processor (5), and well heater and thermopair (4) are fixed on the bottom of ceramic bases (1), constitutes resistance sensor;
B, with light source (6) wavelength coverage above the light emitting diode between the 200-800 nm, Xe lamp, Hg lamp or LASER Light Source are fixed on the sensor that step a makes, sensor is placed the NO that contains concentration known 2In the atmosphere, in room temperature to 500 ℃, at light source (6) 0-100 W/m 2Under the light intensity condition, irradiation sensitive material (3) is signal with the resistance variations of sensitive material (3), and sensor is demarcated;
C, sensor placed the NO that contains unknown concentration 2Atmosphere in, in room temperature to 500 ℃, at light source (6) 0-100 W/m 2Under the light intensity condition, to trace NO 2Carry out Photoelectric Detection.
2. method according to claim 1 is characterized in that being in the step a sensitive material (3) single component semiconductor material nickel oxide, molybdena, cuprous oxide, tungstic acid, tin ash, zinc paste or carbon nano-tube; The heterojunction semiconductor material is tin ash/zinc paste; Composite semiconductor material is yttria-stabilized zirconia or titania/Graphene.
3. method according to claim 1, it is characterized in that the wavelength coverage of step b light source (6) between 200-800 nm, and light source (6) photon energy is more than or equal to the energy gap of the less semiconductor material of heterojunction semiconductor material in the sensitive material (3) or composite semiconductor material energy gap.
4. method according to claim 1 is characterized in that light source (6) uses grating, filter plate, lens and catoptron that light is treated to monochromatic light when sending polychromatic light among step b and the step c.
5. method according to claim 1 is characterized in that light source among the step b (6) is light emitting diode.
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Publication number Priority date Publication date Assignee Title
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CN108195826A (en) * 2017-12-19 2018-06-22 东北大学 Conductance-catalytic luminescence double-channel gas sensor, detection device and its detection method
CN110068588A (en) * 2019-04-28 2019-07-30 济南大学 For detecting NO2Organo-mineral complexing nano material and gas sensor
CN113008943A (en) * 2019-12-20 2021-06-22 财团法人工业技术研究院 Gas sensing device and gas concentration sensing method

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Application publication date: 20131009