CN109521064A - Based on WO3The room temperature NO of hollow sphere2Sensor and preparation method thereof - Google Patents
Based on WO3The room temperature NO of hollow sphere2Sensor and preparation method thereof Download PDFInfo
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- CN109521064A CN109521064A CN201910014213.2A CN201910014213A CN109521064A CN 109521064 A CN109521064 A CN 109521064A CN 201910014213 A CN201910014213 A CN 201910014213A CN 109521064 A CN109521064 A CN 109521064A
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Abstract
One kind being based on WO3The room temperature NO of hollow sphere2Gas sensor and preparation method thereof belongs to gas sensor technical field.The sensor is heater-type structure, by having the alumina ceramic tube substrate of platinum line and gold electrode, coated in the WO on ceramic tube outer surface and gold electrode3Hollow sphere and the nichrome heater strip being placed in ceramic tube form；Nichrome heater strip passes to direct current to provide the operating temperature of sensor, realizes measurement NO by the D.C. resistance resistance value between two gold electrodes in measurement different atmosphere2The function of concentration.Preparation method of the present invention is simple, using size uniformity and is the WO of hollow structure3To NO2Gas is detected, and sensitivity with higher, lower operating temperature, lower Monitoring lower-cut have a good application prospect in terms of environmental monitoring.
Description
Technical field
The invention belongs to gas sensor domains, are related to a kind of based on WO3The room temperature NO of hollow sphere2Sensor and its preparation
Method.
Background technique
With industrialized propulsion, a large amount of fossil fuels are consumed, a large amount of nitrogen dioxide (NO2) gas also therewith by
It has been discharged into air.NO2It endangers huge, can not only cause the environmental problems such as photochemical fog and acid rain, can also damage people
The health of class.Therefore to NO2It is effectively monitored, so that controlling its discharge also just becomes very necessary.Compared to other kinds
The method of class, gas sensor is in NO2Unique advantage that there are many measurement aspects, such as it is at low cost, quick, real-time and convenient.
NO at present2The sensitive material of gas sensor has Si, organic matter, conductor oxidate etc..Based on semiconductor oxide
The NO of object2The features such as sensor has stability good, selective good and high sensitivity, thus have received widespread attention.Relatively
Other metal semiconductor oxides, tungsten oxide (WO3) because tungsten ion valence state can be changed, cause its oxygen content and oxygen defect with environment
Factor changes and changes, so that it is to NO2、H2S、SO2、CO、NH3, ethyl alcohol, the gases sensitivity with higher such as acetone, especially
It is to NO2It is a kind of ideal NO with fabulous response characteristic2Sensitive material.However WO3Material is in detection NO2Gas
In the problems such as that there is operating temperatures is higher, and selectivity is poor, and detection limit is higher.Based on this, the present invention develops one kind in room
The lower work of temperature, can detecte low concentration of NO2WO3Sensor.
Summary of the invention
The present invention provides one kind to be based on WO3The room temperature NO of hollow sphere2Sensor and preparation method thereof, prepared gas
It the features such as body sensor sensitivity with higher, lower Monitoring lower-cut, preferable selectivity, improves gas sensor and exists
Application under room temperature.
In order to achieve the above object, the technical solution adopted by the present invention are as follows:
One kind being based on WO3The room temperature NO of hollow sphere2Sensor, the room temperature NO2Sensor is heater-type structure, by band
There is the ceramic tube substrate of platinum line and gold electrode, coated in the WO on aluminium oxide ceramics tube outer surface and gold electrode3It hollow sphere and sets
In the nichrome heater strip composition in ceramic tube；Nichrome heater strip passes to direct current to provide the work temperature of sensor
Degree realizes measurement NO by the D.C. resistance resistance value between two gold electrodes in measurement different atmosphere2The function of concentration.Wherein, institute
The WO stated3The diameter of hollow sphere is 2~5 μm.
One kind being based on WO3The room temperature NO of hollow sphere2The preparation method of sensor, comprising the following steps:
The first step prepares WO3Hollow sphere
(1) sodium tungstate is dissolved in deionized water, uniform solution is obtained after ultrasonic 10min, adds sodium oxalate later,
The salt acid for adjusting pH value that 6M is added dropwise after 10min is stirred to 0.2~3.0, continues to stir 10min later；Every 25~35ml
It is corresponding that 0.40~0.60g sodium tungstate, 0.10~0.20g sodium oxalate is added in deionized water.
(2) above-mentioned solution being transferred in water heating kettle, is subsequently placed into baking oven, baking oven parameter setting is 150~180 DEG C,
10~for 24 hours；
(3) after reaction, product deionized water and ethyl alcohol alternating centrifugal are washed, obtained product in an oven into
Row drying, drying temperature are 40~80 DEG C, and drying time is 8~12h；2 are calcined under the conditions of being placed on 400~600 DEG C again
~3h, obtains WO3Material, WO3The diameter of hollow sphere is 2~5 μm.
Second step prepares room temperature NO using heater-type structure2Sensor
(1) WO that the first step is prepared3Material and ethyl alcohol 0.2~0.4:1 in mass ratio are uniformly mixed to form slurry；
The slurry is coated uniformly on the surface of the alumina ceramic tube with platinum line and gold electrode, makes it that gold electrode be completely covered；
And platinum filament wire is drawn on gold electrode；
(2) WO will have been coated3The alumina ceramic tube of hollow sphere is sintered 2~5h at 300~600 DEG C, then by ni-Cd
Heating coil passes through inside alumina ceramic tube, passes to direct current to provide operating temperature；Pass through platinum filament wire again for aluminium oxide
Ceramic tube is welded on general heater-type hexagonal pedestal；
(3) finally by sensor aging 5~7 days in 50~150 DEG C of air environments, to obtain WO3Base NO2Gas passes
Sensor.
Air-sensitive performance test is carried out later, and test condition is room temperature, tests nitrogen dioxide (NO2) gas concentration is from 25ppb
~1000ppb.
The beneficial effects of the present invention are:
(1) WO that the present invention is synthesized using one step hydro thermal method3Hollow sphere has than more uniform size distribution, preparation side
Method is simple, to develop high performance NO2Gas sensor provides a kind of effective material.
(2) present invention uses the WO of size uniformity3Hollow sphere is for NO2Gas has higher sensitivity.
(3) sensor developed has lower operating temperature, can be used at room temperature；With lower Monitoring lower-cut,
Monitoring lower-cut can achieve 25ppb；With preferable stability and reliability.
(4) WO that the present invention makes3Base NO2Gas sensor manufacture craft is simple, low in cost, is suitble to industrial batch
Upper production.There is good application prospect in terms of environment measuring.
Detailed description of the invention
Fig. 1 is WO prepared by the embodiment of the present invention 33The SEM (a) and (b) of hollow sphere.
Fig. 2 is the WO of the embodiment of the present invention 3 under room temperature3Base NO2Gas sensitivity and NO2Between concentration
Curve graph.
Specific embodiment
Below with reference to embodiment, the present invention will be further described in detail, but this explanation will not be constituted to of the invention
Limitation.
Embodiment 1
1. 0.40g sodium tungstate is dissolved in 25ml deionized water first, uniform solution is obtained after ultrasonic 10min, later
The salt acid for adjusting pH value for instilling 6M after 0.20g sodium oxalate stirring 10min is added to 0.2, continues to stir 10min later；
2. above-mentioned solution is transferred in the water heating kettle of 50ml, it is subsequently placed into baking oven, baking oven parameter setting is 150 DEG C,
10h；
3. after reaction, product deionized water and ethyl alcohol alternating centrifugal are washed, obtained product in an oven into
Row drying, 60 DEG C of dry 12h.3h is calcined at 600 DEG C later, obtains WO3Material.
4. material made from 0.4mg and 1mg dehydrated alcohol is taken to be uniformly mixed to form slurry.Appropriate slurry is dipped with hairbrush to apply
Commercially available ceramic tube outer surface is overlayed on, makes it that the gold electrode of outer surface be completely covered.
5. coated ceramic tube is sintered 3h at 300 DEG C, then nickel-cadmium heating coil is passed through in ceramic tube
Portion passes to direct current to provide operating temperature.Ceramic tube is welded on general heater-type hexagonal pedestal finally by platinum filament wire
On, to obtain WO3Base NO2Sensor.
6. finally by sensor aging 5 days in 80 DEG C of air environments, for use.
7. NO of the test sensor to 25ppb to 1000ppb at room temperature2Sensitivity.
Embodiment 2
1. 0.45g sodium tungstate is dissolved in 30ml deionized water first, uniform solution is obtained after ultrasonic 10min, later
The salt acid for adjusting pH value for instilling 6M after 0.15g sodium oxalate stirring 10min is added to 0.2, continues to stir 10min later；
2. above-mentioned solution is transferred in the water heating kettle of 50ml, it is subsequently placed into baking oven, baking oven parameter setting is 160 DEG C,
12h；
3. after reaction, product deionized water and ethyl alcohol alternating centrifugal are washed, obtained product in an oven into
Row drying, 40 DEG C of dry 8h.2h is calcined at 500 DEG C later, obtains WO3Material.
4. material made from 0.4mg and 1mg dehydrated alcohol is taken to be uniformly mixed to form slurry.Appropriate slurry is dipped with hairbrush to apply
Commercially available ceramic tube outer surface is overlayed on, makes it that the gold electrode of outer surface be completely covered.
5. coated ceramic tube is sintered 2h at 500 DEG C, then nickel-cadmium heating coil is passed through in ceramic tube
Portion passes to direct current to provide operating temperature.Ceramic tube is welded on general heater-type hexagonal pedestal finally by platinum filament wire
On, to obtain WO3Base NO2Sensor.
6. finally by sensor aging 7 days in 50 DEG C of air environments, for use.
7. NO of the test sensor to 25ppb to 1000ppb at room temperature2Sensitivity.
Embodiment 3
1. 0.45g sodium tungstate is dissolved in 30ml deionized water first, uniform solution is obtained after ultrasonic 10min, later
The salt acid for adjusting pH value for instilling 6M after 0.15g sodium oxalate stirring 10min is added to 0.7, continues to stir 10min later；
2. above-mentioned solution is transferred in the water heating kettle of 50ml, it is subsequently placed into baking oven, baking oven parameter setting is 160 DEG C,
12h；
3. after reaction, product deionized water and ethyl alcohol alternating centrifugal are washed, obtained product in an oven into
Row drying, 40 DEG C of dry 8h.2h is calcined at 500 DEG C later, obtains WO3Material.
4. material made from 0.4mg and 1mg ethyl alcohol is taken to be uniformly mixed to form slurry.Appropriate slurry is dipped with hairbrush to be coated in
Commercially available ceramics tube outer surface, makes it that the gold electrode of outer surface be completely covered.
5. coated ceramic tube is sintered 2h at 500 DEG C, then nickel-cadmium heating coil is passed through in ceramic tube
Portion passes to direct current to provide operating temperature.Ceramic tube is welded on general heater-type hexagonal pedestal finally by platinum filament wire
On, to obtain WO3Base NO2Sensor.
6. finally by sensor aging 7 days in 50 DEG C of air environments, for use.
7. NO of the test sensor to 25ppb to 1000ppb at room temperature2Sensitivity.
As shown in Fig. 1 (a), the WO for preparing3For hollow sphere size than more uniform, the diameter of each hollow ball is 2~5 μm,
Some broken hollow balls can be found by examining.Fig. 1 (b) gives the enlarged drawing of hollow ball, this is also to prove WO3It is hollow
Structure provides direct proof.Fig. 2 lists the WO of preparation3Base NO2Gas sensor sensitivity at room temperature and NO2It is dense
The curve graph of degree.It is worth noting that sensor NO that can be detected2Concentration limit is 25ppb.
Embodiment 4
1. 0.60g sodium tungstate is dissolved in 35ml deionized water first, uniform solution is obtained after ultrasonic 10min, later
The salt acid for adjusting pH value for instilling 6M after 0.10g sodium oxalate stirring 10min is added to 1.3, continues to stir 10min later；
2. above-mentioned solution is transferred in the water heating kettle of 50ml, it is subsequently placed into baking oven, baking oven parameter setting is 180 DEG C,
24h；180-24
3. after reaction, product deionized water and ethyl alcohol alternating centrifugal are washed, obtained product in an oven into
Row drying, 80 DEG C of dry 10h.3h is calcined at 400 DEG C later, obtains WO3Material.
4. material made from 0.2mg and 1mg ethyl alcohol is taken to be uniformly mixed to form slurry.Appropriate slurry is dipped with hairbrush to be coated in
Commercially available ceramics tube outer surface, makes it that the gold electrode of outer surface be completely covered.
5. coated ceramic tube is sintered 5h at 600 DEG C, then nickel-cadmium heating coil is passed through in ceramic tube
Portion passes to direct current to provide operating temperature.Ceramic tube is welded on general heater-type hexagonal pedestal finally by platinum filament wire
On, to obtain WO3Base NO2Sensor.
6. finally by sensor aging 6 days in 150 DEG C of air environments, for use.
7. NO of the test sensor to 25ppb to 1000ppb at room temperature2Sensitivity.
Embodiment 5
1. 0.45g sodium tungstate is dissolved in 30ml deionized water first, uniform solution is obtained after ultrasonic 10min, later
The salt acid for adjusting pH value for instilling 6M after 0.15g sodium oxalate stirring 10min is added to 1.3, continues to stir 10min later；
2. above-mentioned solution is transferred in the water heating kettle of 50ml, it is subsequently placed into baking oven, baking oven parameter setting is 160 DEG C,
12h；
3. after reaction, product deionized water and ethyl alcohol alternating centrifugal are washed, obtained product in an oven into
Row drying, 40 DEG C of dry 8h.2h is calcined at 500 DEG C later, obtains WO3Material.
4. material made from 0.4mg and 1mg ethyl alcohol is taken to be uniformly mixed to form slurry.Appropriate slurry is dipped with hairbrush to be coated in
Commercially available ceramics tube outer surface, makes it that the gold electrode of outer surface be completely covered.
5. coated ceramic tube is sintered 2h at 500 DEG C, then nickel-cadmium heating coil is passed through in ceramic tube
Portion passes to direct current to provide operating temperature.Ceramic tube is welded on general heater-type hexagonal pedestal finally by platinum filament wire
On, to obtain WO3Base NO2Sensor.
6. finally by sensor aging 7 days in 50 DEG C of air environments, for use.
7. NO of the test sensor to 25ppb to 1000ppb at room temperature2Sensitivity.
Embodiment 6
1. 0.50g sodium tungstate is dissolved in 30ml deionized water first, uniform solution is obtained after ultrasonic 10min, later
The salt acid for adjusting pH value for instilling 6M after 0.15g sodium oxalate stirring 10min is added to 2.2, continues to stir 10min later；
2. above-mentioned solution is transferred in the water heating kettle of 50ml, it is subsequently placed into baking oven, baking oven parameter setting is 160 DEG C,
18h；
3. after reaction, product deionized water and ethyl alcohol alternating centrifugal are washed, obtained product in an oven into
Row drying, 60 DEG C of dry 12h.2.5h is calcined at 500 DEG C later, obtains WO3Material.
4. material made from 0.2mg and 1mg ethyl alcohol is taken to be uniformly mixed to form slurry.Appropriate slurry is dipped with hairbrush to be coated in
Commercially available ceramics tube outer surface, makes it that the gold electrode of outer surface be completely covered.
5. coated ceramic tube is sintered 4h at 400 DEG C, then nickel-cadmium heating coil is passed through in ceramic tube
Portion passes to direct current to provide operating temperature.Ceramic tube is welded on general heater-type hexagonal pedestal finally by platinum filament wire
On, to obtain WO3Base NO2Sensor.
6. finally by sensor aging 7 days in 100 DEG C of air environments, for use.
7. NO of the test sensor to 25ppb to 1000ppb at room temperature2Sensitivity.
Embodiment 7
1. 0.45g sodium tungstate is dissolved in 30ml deionized water first, uniform solution is obtained after ultrasonic 10min, later
The salt acid for adjusting pH value for instilling 6M after 0.15g sodium oxalate stirring 10min is added to 2.2, continues to stir 10min later；
2. above-mentioned solution is transferred in the water heating kettle of 50ml, it is subsequently placed into baking oven, baking oven parameter setting is 160 DEG C,
12h；
3. after reaction, product deionized water and ethyl alcohol alternating centrifugal are washed, obtained product in an oven into
Row drying, 40 DEG C of dry 8h.3h is calcined at 400 DEG C later, obtains WO3Material.
4. material made from 0.4mg and 1mg ethyl alcohol is taken to be uniformly mixed to form slurry.Appropriate slurry is dipped with hairbrush to be coated in
Commercially available ceramics tube outer surface, makes it that the gold electrode of outer surface be completely covered.
5. coated ceramic tube is sintered 2h at 500 DEG C, then nickel-cadmium heating coil is passed through in ceramic tube
Portion passes to direct current to provide operating temperature.Ceramic tube is welded on general heater-type hexagonal pedestal finally by platinum filament wire
On, to obtain WO3Base NO2Sensor.
6. finally by sensor aging 7 days in 50 DEG C of air environments, for use.
7. NO of the test sensor to 25ppb to 1000ppb at room temperature2Sensitivity.
Embodiment 8
1. 0.45g sodium tungstate is dissolved in 30ml deionized water first, uniform solution, Zhi Houjia are obtained after ultrasonic 5min
Enter the salt acid for adjusting pH value for instilling 6M after 0.15g sodium oxalate stirring 10min to 3.0, continues to stir 10min later；
2. above-mentioned solution is transferred in the water heating kettle of 50ml, it is subsequently placed into baking oven, baking oven parameter setting is 160 DEG C,
12h；
3. after reaction, product deionized water and ethyl alcohol alternating centrifugal are washed, obtained product in an oven into
Row drying, 60 DEG C of dry 12h.2.5h is calcined at 500 DEG C later, obtains WO3Material.
4. material made from 0.2mg and 1mg ethyl alcohol is taken to be uniformly mixed to form slurry.Appropriate slurry is dipped with hairbrush to be coated in
Commercially available ceramics tube outer surface, makes it that the gold electrode of outer surface be completely covered.
5. coated ceramic tube is sintered 2h at 500 DEG C, then nickel-cadmium heating coil is passed through in ceramic tube
Portion passes to direct current to provide operating temperature.Ceramic tube is welded on general heater-type hexagonal pedestal finally by platinum filament wire
On, to obtain WO3Base NO2Sensor.
6. finally by sensor aging 7 days in 80 DEG C of air environments, for use.
7. NO of the test sensor to 25ppb to 1000ppb at room temperature2Sensitivity.
Embodiment 9
1. 0.45g sodium tungstate is dissolved in 30ml deionized water first, uniform solution is obtained after ultrasonic 10min, later
The salt acid for adjusting pH value for instilling 6M after 0.15g sodium oxalate stirring 10min is added to 3.0, continues to stir 10min later；
2. above-mentioned solution is transferred in the water heating kettle of 50ml, it is subsequently placed into baking oven, baking oven parameter setting is 160 DEG C,
12h；
3. after reaction, product deionized water and ethyl alcohol alternating centrifugal are washed, obtained product in an oven into
Row drying, 40 DEG C of dry 8h.2h is calcined at 500 DEG C later, obtains WO3Material.
4. material made from 0.3mg and 1mg ethyl alcohol is taken to be uniformly mixed to form slurry.Appropriate slurry is dipped with hairbrush to be coated in
Commercially available ceramics tube outer surface, makes it that the gold electrode of outer surface be completely covered.
5. coated ceramic tube is sintered 2h at 500 DEG C, then nickel-cadmium heating coil is passed through in ceramic tube
Portion passes to direct current to provide operating temperature.Ceramic tube is welded on general heater-type hexagonal pedestal finally by platinum filament wire
On, to obtain WO3Base NO2Sensor.
6. finally by sensor aging 7 days in 50 DEG C of air environments, for use.
7. NO of the test sensor to 25ppb to 1000ppb at room temperature2Sensitivity.
Table 1: gas sensor is in 200ppb NO2In atmosphere, the relationship of sensitivity and pH value
(sensitivity S=Rg/Ra, wherein the aerial resistance of Ra representative sensor, Rg are sensor under test gas
Resistance value)
| Embodiment | PH value | Sensitivity S (Rg/Ra) |
| Embodiment 2 | 0.2 | 2.1 |
| Embodiment 3 | 0.7 | 7.6 |
| Embodiment 5 | 1.3 | 1.4 |
| Embodiment 7 | 2.2 | 1.0 |
| Embodiment 9 | 3.0 | 1.0 |
Embodiment described above only expresses embodiments of the present invention, and but it cannot be understood as to the invention patent
Range limitation, it is noted that for those skilled in the art, without departing from the inventive concept of the premise, also
Several modifications and improvements can be made, these are all belonged to the scope of protection of the present invention.
Claims (5)
1. one kind is based on WO3The room temperature NO of hollow sphere2Sensor, which is characterized in that the room temperature NO2Sensor is heater-type
Structure, by having the ceramic tube substrate of platinum line and gold electrode, coated in the WO on aluminium oxide ceramics tube outer surface and gold electrode3It is empty
Bulbus cordis and the nichrome heater strip being placed in ceramic tube form；Nichrome heater strip passes to direct current to provide sensor
Operating temperature realizes measurement NO by the D.C. resistance resistance value between two gold electrodes in measurement different atmosphere2The function of concentration.
2. according to claim 1 a kind of based on WO3The room temperature NO of hollow sphere2Sensor, which is characterized in that the WO3
The diameter of hollow sphere is 2~5 μm.
3. one kind is based on WO3The room temperature NO of hollow sphere2The preparation method of sensor, which comprises the following steps:
The first step prepares WO3Hollow sphere
(1) sodium tungstate is dissolved in deionized water, obtains uniform solution after ultrasound, adds sodium oxalate later, dripped after stirring
Add salt acid for adjusting pH value to 0.2~3.0, continues to stir later；It is corresponding to be added 0.40 in every 25~35ml deionized water
~0.60g sodium tungstate, 0.10~0.20g sodium oxalate；
(2) above-mentioned solution is transferred in water heating kettle, is subsequently placed into baking oven, baking oven parameter setting be 150~180 DEG C, 10~
24h；
(3) after reaction, product deionized water and ethyl alcohol alternating centrifugal are washed, obtained product is done in an oven
It is dry；2~3h is calcined under the conditions of being placed on 400~600 DEG C again, obtains WO3Material；
Second step prepares room temperature NO using heater-type structure2Sensor
(1) WO that the first step is prepared3Material and ethyl alcohol are uniformly mixed to form slurry；The slurry is coated uniformly on and is had
On the surface of the alumina ceramic tube of platinum line and gold electrode, make it that gold electrode be completely covered；And platinum filament is drawn on gold electrode and is led
Line；
(2) WO will have been coated3The alumina ceramic tube of hollow sphere is sintered 2~5h at 300~600 DEG C, then by ni-Cd heater wire
Circle passes to direct current inside alumina ceramic tube to provide operating temperature；Pass through platinum filament wire again for alumina ceramic tube
It is welded on general heater-type pedestal；
(3) sensor is obtained into WO aging 5~7 days in 50~150 DEG C of air environments3Base NO2Gas sensor.
4. preparation method according to claim 3, which is characterized in that baking oven described in the first step step (1)
Drying temperature is 40~80 DEG C, and drying time is 8~12h.
5. preparation method according to claim 3 or 4, which is characterized in that WO described in the first step step (1)3
Material and ethyl alcohol mass ratio are 0.2~0.4:1.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112408484A (en) * | 2020-11-23 | 2021-02-26 | 杭州富通电线电缆有限公司 | Tungsten trioxide hollow ball, preparation method thereof and application thereof in cable sheath |
| CN113189154A (en) * | 2021-05-27 | 2021-07-30 | 扬州大学 | Room-temperature low-concentration hydrogen sulfide gas-sensitive material and preparation method thereof |
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