CN101929958A - High-sensitivity photosensitive gas sensor and preparation method thereof - Google Patents
High-sensitivity photosensitive gas sensor and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-sensitivity photosensitive gas sensor and a preparation method thereof. In a photosensitive gas sensor made of a gas sensitive material, a photocatalyst is introduced to improve the gas sensitivity of a sensitive body, namely a photocatalyst-gas sensitive function composite oxide semiconductor is taken as the sensitive body, on the one hand, the gas sensitive material has good response to gas to be tested, and on the other hand, the photocatalyst absorbs ultraviolet light to the largest extent; and the combined action results in improvement of illumination efficiency and gas sensitive efficiency of the sensitive body, and the sensitivity of the gas sensor is improved finally. Compared with sensors made of a pure gas sensitive material, a sensor made of a sensitive body in which the mass ratio of zinc dioxide to stannic oxide is 3:7 has the sensitivity to 100ppm ethanol gas at 250DEG C improved from 4.3 to 10, and a sensor made of a sensitive body in which the mass ratio of titanium dioxide to stannic oxide is 3:7 has the sensitivity to 100ppm ethanol gas at room temperature improved from 9 to 16.
Description
Technical field
The invention belongs to metal-oxide semiconductor (MOS) gas sensor technical field, be specifically related to a kind of high-sensitivity photosensitive gas sensor and preparation method thereof.
Background technology
The nearly working and room temperature of realizing the metal-oxide semiconductor (MOS) gas sensor is an important directions in gas sensor field always.Present studies show that ultraviolet excitation is most possibly realized the working and room temperature of metal-oxide semiconductor (MOS) gas sensor.
The metal-oxide semiconductor (MOS) gas sensor is the polycrystalline sintered body that is made of great number of grains, and during working sensor, electronics must pass crystal boundary potential barrier and surface depletion layer during from a crystal grain to another crystal grain.Optical excitation can improve the number of charge carrier in the semiconductor, reduces the crystal boundary potential barrier, improves the mobility of charge carrier rate, thereby makes gas sensor at room temperature just have better response to gas to be measured.
Yet the research of light sensitizing type gas sensor also is in the starting stage, main research is to be the sensor of sensitive body with the single oxide at present, the character and the light efficiency of sensitive body are closely related, if can improve the light efficiency of sensitive body, then can improve the gas sensing property of light sensitizing type gas sensor.
Summary of the invention
In order to solve the low problem of sensitivity under the metal-oxide semiconductor (MOS) gas sensor low temperature, the invention provides a kind of is the light sensitizing type gas sensor and preparation method thereof of sensitive body with photocatalyst-gas-sensing function composite oxide semiconductor.
The structure of traditional metal-oxide semiconductor (MOS) gas sensor is made up of substrate 1, electrode 2, well heater 3, sensitive body 4 and ultraviolet source 5 as shown in Figure 1.The invention is characterized in that being is sensitive body 4 with photocatalyst-gas-sensing function composite oxide semiconductor, gas sensitive has been realized the good response to gas to be measured on the one hand, photocatalyst has been realized the absorption to the maximum possible of ultraviolet light on the other hand, the result of combined action has improved the light efficiency and the air-sensitive efficient of sensitive body, the sensitivity that has finally improved gas sensor.
Principle of the present invention as shown in Figure 2, it is the transfer process of photogenerated charge in photocatalyst-gas-sensing function composite oxide semiconductor sensitive body 4, the ultraviolet light that shines on the sensitive body is at first absorbed by photocatalyst, in photocatalyst, produce photogenerated charge, since exist between gas sensitive and the photocatalyst can be with poor, therefore the photogenerated charge that produces can enter in the gas sensitive at photocatalyst and air-sensitive crystal boundary of material place, play absorption that promotes oxygen in the air and the effect that reduces interface potential barrier, therefore improved the gas sensitivity under the sensitive body low temperature.
Be fit to do the SnO that has of gas sensitive
2, Fe
3O
4, In
2O
3, WO
3Deng, being fit to photocatalyst has ZnO or TiO
2Deng.
It is the sensitive body of gas sensor that the present invention has proposed with photocatalyst-gas-sensing function composite oxide semiconductor first, has improved the sensitivity of the nearly working and room temperature of light sensitizing type gas sensor.
A kind of high-sensitivity photosensitive gas sensor of the present invention, its preparation process is as follows:
1, prepares photocatalyst nano particle and air-sensitive material nano particle respectively with sluggish precipitation, prepared nano particle is spheroidal particle, then with photocatalyst nano particle and air-sensitive material nano mix particles, thereby obtain photocatalyst-gas-sensing function composite oxide semiconductor as sensitive body, the mass content of photocatalyst is 10%~90% in the sensitive body, and all the other are gas sensitive;
The gas sensitive nano particle is SnO
2, Fe
3O
4, In
2O
3Or WO
3Nano particle, photocatalyst nano particle are ZnO or TiO
2, wherein, the mean diameter of ZnO nano particle is about 5~30 nanometers, TiO
2The mean diameter of nano particle is 10~30 nanometers, SnO
2The mean diameter of nano particle is 10~40 nanometers; Photocatalyst can be a kind of nano particle of photocatalyst, also can be the mixing of multiple photocatalyst nano particle; Gas sensitive can be a kind of nano particle of gas sensitive, also can be the mixing of multiple air-sensitive nano particle;
Preferably, in the sensitive body material, the mass content of photocatalyst nano particle is 15~75%; Further preferred, the mass content of ZnO nano particle is 15~50% in the sensitive body material, and all the other are the gas sensitive nano particle; TiO in the sensitive body material
2The mass content of nano particle is 35~65%, and all the other are the gas sensitive nano particle;
2, choosing pipe range is that 3~8mm, external diameter are that 1.0~1.4mm, internal diameter are the Al of 0.6~0.8mm
2O
3Ceramic pipe is as substrate 1, with gold ring and platinum filament as electrode 2;
3, grind after 0.1~0.5 gram sensitive body material dissolves of step 1 preparation is in deionized water, making it form concentration is the pasty liquid of 50~500 mg/ml, adopts the method for spin coating pasty liquid evenly to be coated in the Al that has electrode 2 then
2O
3On the outside surface of ceramic pipe substrate 1, form thickness and be 200~600 microns sensitive body 4, treated to send into after air-dry in the muffle furnace under 450~650 ℃ of temperature conditions sintering 1~5 hour, naturally cool to room temperature;
4, be that 25~40 Ω, the number of turn are that the Ni~Cr heater coil of 30~50 circles passes the cooled ceramic pipe that is coated with sensitive body 4 as well heater 3 then with resistance, promptly preparing structure of the present invention is the high-sensitivity photosensitive gas sensor of the nearly working and room temperature of ceramic pipe substrate 1/ electrode 2/ sensitive body 4/ ultraviolet source 5.
Wherein ultraviolet source 5 is that power is the commercially available ultraviolet light-emitting diode of 60 milliwatts.
Under the 100ppm alcohol atmosphere, test the performance of gas sensor of the present invention, comprise the sensitivity and the illumination front and back sensitivity rate of change of working temperature, illumination front and back.
Table 1: the performance parameter of the sensor of each example preparation
? | Working temperature (℃) | Sensitivity (S before the illumination D)? | Sensitivity (S after the illumination L)? | Sensitivity rate of change (S before and after the illumination L-S D)/S D(%)? |
Comparative Examples 1 | 250? | 2.1? | 2.8? | 33? |
Comparative Examples 2 | 250? | 5.5? | 11.5? | 109? |
Comparative Examples 3 | 250? | 6.1? | 9.0? | 48? |
Embodiment 1 | 250? | 4.8? | 5.1? | 6.2? |
|
250? | 4.3? | 10.0? | 132? |
|
250? | 6.4? | 7.3? | 14? |
|
250? | 5.0? | 6.2? | 24? |
|
250? | 6.7? | 8.4? | 25? |
|
Room temperature | 1.2? | 1.5? | 25? |
Embodiment 7 | Room temperature | 2.1? | 3.5? | 67? |
|
Room temperature | 9.0? | 16.0? | 78? |
|
Room temperature | 2.0? | 2.3? | 15? |
Table 1 has been listed Comparative Examples 1,2, and 3 and the performance parameter of the sensor of embodiment 1,2,3,4,5,6,7,8,9 preparation, comprise sensitivity rate of change before and after sensitivity before and after working temperature, the illumination and the illumination.The sensitivity S of gas sensor is defined as the ratio of the resistance value Rg in airborne resistance value Ra and the gas to be measured, i.e. S=Ra/Rg.
As can be seen from Table 1: the tin ash sensitive material of doping photocatalyst during as sensitive body gas sensor for the purer tin ash of the sensitivity of alcohol gas highly sensitive for alcohol gas during as sensitive body.When photocatalyst is zinc oxide, when the quality of zinc oxide account for total sensitive body 30% the time, after the illumination sensor 250 ℃ down during work the peak response for the 100ppm alcohol gas be 10, than having increased by 132% before the illumination; When photocatalyst is titania, when the quality of titania account for total sensitive body 50% the time, sensor can at room temperature be worked after the illumination, this moment, the maximum room temperature sensitivity for the 100ppm alcohol gas was 16, than having increased by 78% before the illumination.Equally, also as can be seen, the sensitivity difference of sensor during the photocatalyst of doping different content, the mass content of doping zinc oxide are performance the best of 30% o'clock sensor from Fig. 3; Titania-doped mass content is 50% o'clock, performance the best of sensor.
The sensitivity curve of gas sensor when Fig. 3 is the different content photocatalyst.
Beneficial effect: the method for designing that the invention provides a kind of high-sensitivity photosensitive gas sensor sensitive body.Be specially in the light sensitizing type gas sensor that with the tin ash is gas sensitive, introduce light efficiency and air-sensitive efficient that photocatalyst titania or zinc oxide improve sensitive body.With photocatalyst-gas-sensing function composite oxide semiconductor is sensitive body 4, and gas sensitive has been realized the good response to gas to be measured on the one hand; Photocatalyst has been realized the absorption to the maximum possible of ultraviolet light on the other hand, has improved the light efficiency and the air-sensitive efficient of gas sensitive, the room temperature sensitivity that has finally improved gas sensor.The material of doping photocatalyst during as sensitive body gas sensor for the purer tin ash of the sensitivity of alcohol gas highly sensitive for alcohol gas.When photocatalyst is zinc paste, when the quality of zinc paste account for total sensitive body gross mass 30% the time, sensor has increased to 10 to the sensitivity of the alcohol gas of 100ppm by 4.3 when at room temperature working after the illumination, sensitivity has increased by 132% before than illumination; When photocatalyst is titania, when the quality of titania account for the sensitive body gross mass 50% the time, after the illumination 250 ℃ down during work sensor the sensitivity of the alcohol gas of 100ppm has been increased to 16 by 9, sensitivity has increased by 78% before than illumination.
Description of drawings
Fig. 1: of the present invention is the light sensitizing type gas sensor configuration synoptic diagram of sensitive body with photocatalyst-gas-sensing function composite oxide semiconductor;
Fig. 2: the transfer process synoptic diagram of photogenerated charge in photocatalyst-gas-sensing function composite oxide semiconductor sensitive body;
Fig. 3: the sensitivity curve of gas sensor during different photocatalyst content in the sensitive body;
(a) be with ZnO-SnO
2As sensitive body, be (b) with TiO
2-SnO
2As sensitive body;
Wherein, curve A is sensitivity before the illumination; Curve B is sensitivity after the illumination.
Embodiment
Comparative Examples 1:
Disposing 100 milliliters, concentration is the butter of tin (SnCl of 0.2 mol
45H
2O, analyze pure, Chemical Reagent Co., Ltd., Sinopharm Group) deionized water solution, use weak aqua ammonia (to analyze pure then, Beijing new light chemical reagent work, the volume ratio of ammoniacal liquor and deionized water is 1: 10) carry out titration as precipitation agent, the pH that is titrated to reaction system is till 3, through getting rid of foreign ion after 7~8 eccentric cleaning, obtain pure precipitation Sn (OH) then
4Sintering 2 hours under 450 ℃ of temperature conditions at last, obtaining 3 gram mean grain sizes is the tin ash (SnO of 30 nanometers
2) nanoparticle powder.
Choosing pipe range is that 4mm, wall thickness are that 0.2mm, external diameter (diameter) are the Al of 0.8mm for 1.2mm, internal diameter (diameter)
2O
3Ceramic pipe is a substrate 1, is electrode 2 (purchasing in the Siping City semiconductor factory) with gold ring and platinum filament.With SnO
2Powder is placed in the deionized water and grinds, and the ratio of adjusting deionized water makes it form pasty state, adopts the method for spin coating that it evenly is coated in Al
2O
3On the ceramic pipe, treat to send into after air-dry in the muffle furnace, naturally cool to room temperature 600 ℃ of sintering 2 hours.The Ni-Cr heater coil 3 of 30 Ω is passed the cooled ceramic pipe that has sensitive body 4 as well heater, promptly obtain gas sensor.The ultraviolet source 5 that test is used is that power is the commercially available ultraviolet light-emitting diode of 60 milliwatts.
Comparative Examples 2:
Preparing 100 milliliters, concentration is the zinc acetate (Zn (CH of 0.1 mol
3COO)
22H
2O, analyze pure, the Shantou Xilong Chemical Factory, Guangdong) aqueous solution, carry out titration with 0.5 mol potassium hydroxide (analyze pure, Beijing Chemical Plant) solution as precipitation agent, the PH when reaction finishes is 10, to precipitate water and clean 7~8 times, obtain clean precipitation Zn (OH)
2450 ℃ of sintering 2 hours, obtaining quality is 0.8 gram, mean grain size is zinc paste (ZnO) powder of 20 nanometers.
Device architecture and preparation method are with Comparative Examples 1, and different is is the sensitive body material with ZnO.
Comparative Examples 3:
With 10 milliliters of butyl titanate (Ti (OC
4H
9)
4Chemical pure, Tianjin recovery fine chemistry industry research institute) absolute ethyl alcohol that is dissolved in 150 milliliters (is analyzed pure, the Beijing Chemical Plant) in the solvent, 80 ℃ of following heated and stirred 1 hour, surplus solution is put into 60 ℃ of following evaporates to dryness of air dry oven, then 500 ℃ of following sintering 2 hours, obtaining quality is 2 grams, and mean grain size is the titania (TiO of 10 nanometers
2) powder.
Device architecture and preparation method are with Comparative Examples 1, and different is with TiO
2Be the sensitive body material.
Embodiment 1:
With the ZnO of method preparation in the Comparative Examples 2, the SnO of method preparation in the Comparative Examples 1
2Mix at 1: 9 according to mass ratio,, add the deionized water wet-milling again and formed pastel in 30 minutes this compound substance dry grinding earlier 2 hours, standby.
Choosing pipe range is that 4mm, wall thickness are that 0.2mm, external diameter are that 1.2mm, internal diameter are the Al of 0.8mm
2O
3Ceramic pipe is a substrate 1, is electrode 2 (purchasing in the Siping City semiconductor factory) with gold ring and platinum filament.The method that adopts spin coating is with ZnO and SnO
2Mass ratio is that 1: 9 pastel evenly is coated in Al
2O
3On the ceramic pipe, treat to send into after air-dry in the muffle furnace, naturally cool to room temperature 600 ℃ of sintering 2 hours.The Ni-Cr heater coil 3 of 30 Ω is passed the cooled ceramic pipe that has sensitive body 4 as well heater, promptly obtain gas sensor.Ultraviolet source 5 is that power is the commercially available ultraviolet light-emitting diode of 60 milliwatts.
Embodiment 2:
Device architecture and preparation method are with embodiment 1, and that different is ZnO and SnO
2Mass ratio is 3: 7.
Embodiment 3:
Device architecture and preparation method are with embodiment 1, and that different is ZnO and SnO
2Mass ratio is 5: 5.
Embodiment 4:
Device architecture and preparation method are with embodiment 1, and that different is ZnO and SnO
2Mass ratio is 7: 3.
Embodiment 5:
Device architecture and preparation method are with embodiment 1, and that different is ZnO and SnO
2Mass ratio is 9: 1.
Embodiment 6:
TiO with method preparation in the Comparative Examples 3
2, the SnO of method preparation in the Comparative Examples 1
2Mix at 1: 9 according to mass ratio,, add the entry wet-milling again and formed pastel in 30 minutes this compound substance dry grinding earlier 2 hours, standby.
Choosing pipe range is that 4mm, wall thickness are that 0.2mm, external diameter are that 1.2mm, internal diameter are the Al of 0.8mm
2O
3Ceramic pipe is a substrate 1, is electrode 2 (purchasing in the Siping City semiconductor factory) with gold ring and platinum filament.The method that adopts spin coating is with TiO
2With SnO
2Mass ratio is that 1: 9 pastel evenly is coated in Al
2O
3On the ceramic pipe, treat to send into after air-dry in the muffle furnace, naturally cool to room temperature 600 ℃ of sintering 2 hours.The Ni-Cr heater coil 3 of 30 Ω is passed the cooled ceramic pipe that has sensitive body 4 as well heater, promptly obtain gas sensor.Ultraviolet source 5 is that power is the commercially available ultraviolet light-emitting diode of 60 milliwatts.
Embodiment 7:
Device architecture and preparation method are with embodiment 6, and that different is TiO
2With SnO
2Mass ratio is 3: 7.
Embodiment 8:
Device architecture and preparation method are with embodiment 6, and that different is TiO
2With SnO
2Mass ratio is 5: 5.
Embodiment 9:
Device architecture and preparation method are with embodiment 6, and that different is TiO
2With SnO
2Mass ratio is 7: 3.
Claims (10)
1. high-sensitivity photosensitive gas sensor, form by substrate (1), electrode (2), well heater (3), sensitive body (4) and ultraviolet source (5), it is characterized in that: be to be sensitive body (4) with photocatalyst-gas-sensing function composite oxide semiconductor, the mass content of photocatalyst is 10%~90% in the sensitive body, and all the other are gas sensitive.
2. a kind of high-sensitivity photosensitive gas sensor as claimed in claim 1 is characterized in that: in the sensitive body material, the mass content of photocatalyst is 15~75%.
3. a kind of high-sensitivity photosensitive gas sensor as claimed in claim 2 is characterized in that: gas sensitive is SnO
2, Fe
3O
4, In
2O
3, WO
3The mixing of one or more in the nano particle, photocatalyst are ZnO or TiO
2In one or both mixing.
4. a kind of high-sensitivity photosensitive gas sensor as claimed in claim 3 is characterized in that: the mass content of ZnO nano particle is 15~50% in the sensitive body material, and all the other are gas sensitive.
5. a kind of high-sensitivity photosensitive gas sensor as claimed in claim 3 is characterized in that: TiO in the sensitive body material
2The mass content of nano particle is 35~65%, and all the other are gas sensitive.
6. the preparation method of the described a kind of high-sensitivity photosensitive gas sensor of claim 1, its preparation process is as follows:
1) prepares photocatalyst nano particle and air-sensitive material nano particle respectively with sluggish precipitation, then with photocatalyst nano particle and air-sensitive material nano mix particles, thereby obtain photocatalyst-gas-sensing function composite oxide semiconductor as sensitive body, the mass content of photocatalyst is 10%~90% in the sensitive body, and all the other are gas sensitive;
2) choosing pipe range is that 3~8mm, external diameter are that 1.0~1.4mm, internal diameter are the Al of 0.6~0.8mm
2O
3Ceramic pipe is as substrate (1), with gold ring and platinum filament as electrode (2);
3) grind after 0.1~0.5 gram sensitive body material dissolves of step 1) preparation is in deionized water, making it form concentration is the pasty liquid of 50~500 mg/ml, adopts the method for spin coating pasty liquid evenly to be coated in the Al that is wound with electrode (2) then
2O
3On the outside surface of ceramic pipe substrate (1), form thickness and be 200~600 microns sensitive body (4), treated to send into after air-dry in the muffle furnace under 450~650 ℃ of temperature conditions sintering 1~5 hour, naturally cool to room temperature;
4) and then with resistance is that 25~40 Ω, the number of turn are that the Ni~Cr heater coil of 30~50 circles passes the cooled ceramic pipe that is coated with sensitive body (4) as well heater (3), promptly prepares high-sensitivity photosensitive gas sensor.
7. the preparation method of a kind of high-sensitivity photosensitive gas sensor as claimed in claim 6, it is characterized in that: in the sensitive body material, the mass content of photocatalyst is 15~75%.
8. the preparation method of a kind of high-sensitivity photosensitive gas sensor as claimed in claim 7, it is characterized in that: gas sensitive is SnO
2, Fe
3O
4, In
2O
3, WO
3The mixing of one or more in the nano particle, photocatalyst are ZnO or TiO
2In one or both mixing.
9. the preparation method of a kind of high-sensitivity photosensitive gas sensor as claimed in claim 8, it is characterized in that: photocatalyst is the ZnO nano particle in the sensitive body material, and its mass content is 15~50%, and all the other are gas sensitive.
10. the preparation method of a kind of high-sensitivity photosensitive gas sensor as claimed in claim 8, it is characterized in that: photocatalyst is TiO in the sensitive body material
2Nano particle, its mass content are 35~65%, and all the other are gas sensitive.
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