CN107884449A - One kind is directed to H2The high gas sensor of selectivity - Google Patents
One kind is directed to H2The high gas sensor of selectivity Download PDFInfo
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Abstract
The present invention relates to one kind to be directed to H2The high gas sensor of selectivity, the gas sensor are heater-type structure, including earthenware, are provided with sensitive material in ceramic tube outer surface, are provided with a pair of gold electrodes on the both sides of sensitive material, heating element heater is provided with the inside of earthenware；The heating element heater is Pt heater strips；The sensitive material is a kind of mixture, including SnO2/MnO2Composite hollow ball and Ni nano-powders.
Description
Technical field
The present invention relates to gas sensor technical field, more particularly to one kind to be directed to H2The high gas sensor of selectivity.
Background technology
At present, with the variation of environmental quality, the application to gas sensor is more and more, specifically in many application sides
Face, the raising to gas sensitivity, job stability and repeatability are also very urgent.Ratio, supervised in air quality
Survey field, improves sensor stability and repeatability can be good at detecting toxic and harmful gas.In the prior art, metal aoxidizes
Thing gas sensor has obtained developing on a large scale very much, for example the material such as indium oxide, tin oxide, tungsten oxide is widely used as gas sensitive,
It has the advantages that low cost, high sensitivity.
Wherein, SnO2Nano material be widely used in lithium ion battery, gas sensor, DSSC with
And the field such as catalysis, at present, it has been prepared for the SnO of various patterns2Nanostructured, such as zero-dimension nano particle, monodimension nano stick,
Nanobelt, nano wire, two-dimensional nano piece and three-dimensional graded structure etc..As a kind of traditional gas sensitive, SnO2Nanometer material
Material can show gas-sensitive property in different gas, and its resistance can form different changes under different atmospheric conditions
Trend.
Although various SnO2Nano material has the gentle body absorption position of big specific surface area, more dynamics model, still
SnO2Gas sensitive is poor to the selectivity of gas, in addition, it is not very high as the utilization rate of sensitive material, such as gas
Molecule is difficult to spread and enter SnO2The deep regions of nano material, the utilization ratio of sensitive body can not be improved very well, this
It is the practical problem for limiting its application.
The content of the invention
Based on above-mentioned technical problem, the present invention is intended to provide a kind of be directed to H2The high gas sensor of selectivity, to solve
Above mentioned problem.
One kind is provided in embodiments of the invention and is directed to H2The high gas sensor of selectivity, the gas sensor are side
Hot type structure, including earthenware, sensitive material is provided with ceramic tube outer surface, a pair of gold medals are provided with the both sides of sensitive material
Electrode, heating element heater is provided with the inside of earthenware；The thickness of the gold electrode is 2mm, and the heating element heater is Pt heater strips；It is described
Sensitive material is a kind of mixture, including SnO2/MnO2Composite hollow ball and Ni nano-powders.
The technical scheme that embodiments of the invention provide can include the following benefits：
In sensor of the invention, the sensitive material is based on SnO2/MnO2Composite hollow ball and Ni nano-powders, are realized
To H2High selectivity, there is unexpected technique effect, it is practical.
The additional aspect of the present invention and advantage will be set forth in part in the description, and will partly become from the following description
Obtain substantially, or recognized by the practice of the present invention.It should be appreciated that the general description and following detailed description of the above are only
It is exemplary and explanatory, the present invention can not be limited.
Brief description of the drawings
Using accompanying drawing, the invention will be further described, but the embodiment in accompanying drawing does not form any limit to the present invention
System, for one of ordinary skill in the art, on the premise of not paying creative work, can also be obtained according to the following drawings
Other accompanying drawings.
Fig. 1 is the cross section structure schematic diagram of gas sensor of the present invention；
1- earthenwares, 2- sensitive materials, 3- gold electrodes.
Embodiment
Here exemplary embodiment will be illustrated in detail, its example is illustrated in the accompanying drawings.Following description is related to
During accompanying drawing, unless otherwise indicated, the same numbers in different accompanying drawings represent same or analogous key element.Following exemplary embodiment
Described in embodiment do not represent and the consistent all embodiments of the present invention.On the contrary, they be only with it is such as appended
The example of the consistent apparatus and method of some aspects being described in detail in claims, of the invention.
Fig. 1 is the structural representation of embodiments of the invention, as shown in figure 1, the gas sensor is heater-type structure, bag
Earthenware 1 is included, sensitive material 2 is provided with the outer surface of earthenware 1, a pair of gold electrodes 3 are provided with the both sides of sensitive material 2,
Heating element heater is provided with the inside of earthenware 1；The thickness of the gold electrode 3 is 2mm, and the heating element heater is Pt heater strips；Wherein, institute
It is a kind of mixture to state sensitive material 2, including SnO2/MnO2Composite hollow ball and Ni nano-powders.
SnO2As a kind of common sensitive material, at present, the SnO based on various structures2Nano material is produced, and it is tied
Structure is constantly adjusting, and performance is also constantly improving.Performance of the microstructure of gas sensitive to gas-sensitive property plays most important
Effect, in the gas sensitive course of work, for object gas while being reacted with sensitive material, it is also in sensitive material
It is diffused, if diffusion rate is too small compared with reaction speed, negative influence will be produced to the sensitivity of sensitive material,
And one kind disclosed in this invention is directed to H2The high gas sensor of selectivity, sensitive material is based on SnO in the gas sensor2/
MnO2Composite hollow spherical structure, the hollow ball structure are prepared by template, hydro-thermal method of carbonaceous polysaccharide microsphere, and it can ensure
The deeper region that sensitive material fully contacts with object gas and enables gas to diffuse into sensitive material, it is quick so as to improve
Feel the utilization ratio of material.
The SnO2/MnO2Composite hollow ball is prepared by template, hydro-thermal method of carbonaceous polysaccharide microsphere, the SnO2/MnO2
The particle diameter of composite hollow ball is 150nm, SnO2With MnO2Mass ratio be 3:2.
Selectivity is to characterize co-existing gases to object gas annoyance level, and for certain gas, sensor has high
Sensitivity, and for other gas, sensor is low to its sensitivity, and such case illustrates that sensor has good selection
Property.Specific to SnO2Nano material, it can all show gas-sensitive property in different gas, and its resistance value is in different gas
Different variation tendencies, therefore, SnO can be formed in atmosphere2Base gas sensor is often poor to the selectivity of object gas.This
Invent in the sensitive material, the composite hollow ball is based on SnO2With MnO2Composite, it enables to reducibility gas H2More
Easily reacted on sensitive material surface, and suppress the reaction of other species and sensitive material, so as to realize selectivity.
Further, SnO is worked as2With MnO2Mass ratio difference when, it is to H2Selectivity it is different, when the mass ratio
For 3:2nd, when sensitive material operating temperature is 200 DEG C, its sensitivity to hydrogen substantially exceeds the reaction to other gases,
With unexpected susceptibility, to H2Show as single selectivity.
In above-mentioned sensitive material, the Ni nano-powders and SnO2/MnO2The mass ratio of composite hollow ball is 1:9, the Ni
The particle diameter of nano-powder is 500nm.
In the sensitive material, in addition to Ni nano-powders, the Ni nano-powders are for MnO2Oxidizing property play and urge
Change acts on, so as to which positive role is played in the raising to sensor selectivity.
In another preferred embodiment, one layer of tin film is additionally provided between the sensitive material and earthenware, should
Tin film is prepared on the earthenware using the method for cold spraying, and the tin film thickness is 500 μm.
One kind disclosed in this invention is directed to H2The high gas sensor of selectivity, in sensitive material and ceramic pipe surface also
Provided with tin film, the tin film is for SnO2/MnO2The selectivity of composite hollow spherical structure plays positive role.
Embodiment
The preparation process of the gas sensor is：
Step 1, prepare carbonaceous polysaccharide microsphere：
5g glucose is dissolved in into 35ml to go in example water to form settled solution, then put it into water heating kettle, by the water
Hot kettle keeps 10h at 190 DEG C, by the precursor liquid ethanol of gained and goes example water to clean repeatedly 5 times, afterwards in 80 DEG C of drying
13h, obtain carbonaceous polysaccharide microsphere；
Step 2, prepare SnO2/MnO2Composite hollow ball：
By 0.2mmol MnCl2·4H2O is dissolved in the solution A that 0.02mol/L is formed in 10ml dimethylformamide；Will
0.4mmol SnCl4·5H2O is dissolved in the solution B that 0.04mol/L is formed in 10ml dimethylformamide；0.3g carbonaceous is more
Sugared microballoon ultrasound, which is dissolved in 50ml dimethylformamide, forms solution C；Then solution A, B are slowly dropped in solution C, together
When continuous magnetic agitation；Then after ultrasonic 30min, mixed solution is placed at room temperature 1 day, then with ethanol and deionized water
Alternating centrifugal is cleaned, and solid mixture is dried into 10h at 70 DEG C；
Step 3, prepare sensitive material：
Ni nano-powders are mixed with the solid mixture after above-mentioned centrifugal drying, ground uniformly, then forge its high temperature
Burn；
Preferably, the high-temperature burning process is：4h is calcined at 240 DEG C respectively, calcines 5h at 510 DEG C；
Step 4, prepare gas sensor：
The surface cold spraying tin film between two gold electrodes being parallel to each other of earthenware, then by after above-mentioned high-temperature calcination
Product with going example water to be well mixed and forming starchiness, be coated onto tin film surface, thickness is 500 μm, in infrared lamp
After lower dry 30min, the earthenware is placed in 400 DEG C of sintering 2h in Muffle furnace, then Pt heater strips are inserted into earthenware,
To provide the operating temperature of sensor, the gas sensor is obtained after welding lead.
Reference examples 1
Compared to embodiment, SnO2With MnO2Mass ratio be 1:1.
Step 1, prepare carbonaceous polysaccharide microsphere：
5g glucose is dissolved in into 35ml to go in example water to form settled solution, then put it into water heating kettle, by the water
Hot kettle keeps 10h at 190 DEG C, by the precursor liquid ethanol of gained and goes example water to clean repeatedly 5 times, afterwards in 80 DEG C of drying
13h, obtain carbonaceous polysaccharide microsphere；
Step 2, prepare SnO2/MnO2Composite hollow ball：
By 0.2mmol MnCl2·4H2O is dissolved in the solution A that 0.02mol/L is formed in 10ml dimethylformamide；Will
0.4mmol SnCl4·5H2O is dissolved in the solution B that 0.04mol/L is formed in 10ml dimethylformamide；0.3g carbonaceous is more
Sugared microballoon ultrasound, which is dissolved in 50ml dimethylformamide, forms solution C；Then solution A, B are slowly dropped in solution C, together
When continuous magnetic agitation；Then after ultrasonic 30min, mixed solution is placed at room temperature 1 day, then with ethanol and deionized water
Alternating centrifugal is cleaned, and solid mixture is dried into 10h at 70 DEG C；
Step 3, prepare sensitive material：
Ni nano-powders are mixed with the solid mixture after above-mentioned centrifugal drying, ground uniformly, then forge its high temperature
Burn；
Preferably, the high-temperature burning process is：4h is calcined at 240 DEG C respectively, calcines 5h at 510 DEG C；
Step 4, prepare gas sensor：
The surface cold spraying tin film between two gold electrodes being parallel to each other of earthenware, then by after above-mentioned high-temperature calcination
Product with going example water to be well mixed and forming starchiness, be coated onto tin film surface, thickness is 500 μm, in infrared lamp
After lower dry 30min, the earthenware is placed in 400 DEG C of sintering 2h in Muffle furnace, then Pt heater strips are inserted into earthenware,
To provide the operating temperature of sensor, the gas sensor is obtained after welding lead.
Reference examples 2
Compared to embodiment, SnO2With MnO2Mass ratio be 2:3.
Step 1, prepare carbonaceous polysaccharide microsphere：
5g glucose is dissolved in into 35ml to go in example water to form settled solution, then put it into water heating kettle, by the water
Hot kettle keeps 10h at 190 DEG C, by the precursor liquid ethanol of gained and goes example water to clean repeatedly 5 times, afterwards in 80 DEG C of drying
13h, obtain carbonaceous polysaccharide microsphere；
Step 2, prepare SnO2/MnO2Composite hollow ball：
By 0.2mmol MnCl2·4H2O is dissolved in the solution A that 0.02mol/L is formed in 10ml dimethylformamide；Will
0.4mmol SnCl4·5H2O is dissolved in the solution B that 0.04mol/L is formed in 10ml dimethylformamide；0.3g carbonaceous is more
Sugared microballoon ultrasound, which is dissolved in 50ml dimethylformamide, forms solution C；Then solution A, B are slowly dropped in solution C, together
When continuous magnetic agitation；Then after ultrasonic 30min, mixed solution is placed at room temperature 1 day, then with ethanol and deionized water
Alternating centrifugal is cleaned, and solid mixture is dried into 10h at 70 DEG C；
Step 3, prepare sensitive material：
Ni nano-powders are mixed with the solid mixture after above-mentioned centrifugal drying, ground uniformly, then forge its high temperature
Burn；
Preferably, the high-temperature burning process is：4h is calcined at 240 DEG C respectively, calcines 5h at 510 DEG C；
Step 4, prepare gas sensor：
The surface cold spraying tin film between two gold electrodes being parallel to each other of earthenware, then by after above-mentioned high-temperature calcination
Product with going example water to be well mixed and forming starchiness, be coated onto tin film surface, thickness is 500 μm, in infrared lamp
After lower dry 30min, the earthenware is placed in 400 DEG C of sintering 2h in Muffle furnace, then Pt heater strips are inserted into earthenware,
To provide the operating temperature of sensor, the gas sensor is obtained after welding lead.
Preferably, the air-sensitive test of gas sensor of the present invention is using static test system in test box, is surveyed
During examination, environment temperature is 25 DEG C；A certain amount of under test gas is injected into test box, under test gas and the air in chamber
Gas sensor of the present invention is put into test box after well mixed.
Medium sensitivity (S) of the present invention is defined as：S=Ra/Rg, wherein, Ra and Rg be respectively gas sensor in atmosphere
With the resistance value under test gas；Since the response time be defined as gas sensor and reached entering under test gas to responsiveness change
To total changing value 90% when required time, since recovery time be defined as gas sensor departing under test gas to response
Degree change reaches the time required during the 90% of total changing value.
For the selectivity of the gas sensor, sensor described in embodiment is tested first respectively 500ppm's
H2、NH3、NO2、CO2In sensitivity, such as table 1 below：
Sensor is respectively in 500ppm H described in the embodiment of table 12、NH3、NO2、CO2In sensitivity
| Embodiment | H2 | NH3 | NO2 | CO2 |
| 150℃ | 19 | 15 | 18 | 12 |
| 200℃ | 36 | 4 | 2 | 3 |
| 250℃ | 26 | 23 | 20 | 18 |
It can be seen that, when the operating temperature of sensor is 200 DEG C, it is in H from table2In sensitivity highest, and
It is in other gas (NH3、NO2、CO2) medium sensitivity with H2Medium sensitivity difference is larger；When senor operating temperature is 150
DEG C or at 250 DEG C, it is in other gas (NH3、NO2、CO2) medium sensitivity with H2Medium sensitivity is suitable, shows it to H2Not
Possesses selectivity, therefore, gas sensor operating temperature of the present invention is 200 DEG C.
Secondly, operating temperature is set as 200 DEG C, tests sensor described in reference examples 1,2 respectively respectively in 500ppm
H2、NH3、NO2、CO2In sensitivity, such as table 2 below：
When the operating temperature of table 2 is 200 DEG C, sensor described in reference examples is respectively in 500ppm H2、NH3、NO2、CO2In
Sensitivity
| H2 | NH3 | NO2 | CO2 | |
| Reference examples 1 | 21 | 16 | 9 | 7 |
| Reference examples 2 | 30 | 23 | 17 | 19 |
It can be seen that in reference examples 1,2, the sensor is to H2、NH3Higher sensitivity is showed, it is by contrast, right
NO2、CO2Sensitivity decrease, but difference is not very big, with reference to table 1, is illustrated in reference examples 1,2, the gas sensing
Device is to H2The selectivity shown has substantial degradation.
Therefore, in sensor of the present invention, the SnO2/MnO2SnO in composite hollow ball2With MnO2Mass ratio to pass
Sensor selectively has large effect, when the mass ratio is 3:When 2, it has higher sensitivity to hydrogen, while can
Guarantee has relatively low sensitivity to other gases, that is to say, that under the mass ratio, sensor sheet of the present invention reveals
Unexpected selectivity.
The preferred mode of the present invention is the foregoing is only, is not intended to limit the invention, it is all in the spiritual and former of the present invention
Within then, any modification, equivalent substitution and improvements made etc., it should be included in the scope of the protection.
Claims (9)
1. one kind is directed to H2The high gas sensor of selectivity, the gas sensor are heater-type structure, including earthenware, are being made pottery
Porcelain tube outer surface is provided with sensitive material, is provided with a pair of gold electrodes on the both sides of sensitive material, is provided with the inside of earthenware
Heating element heater；It is characterized in that：The heating element heater is Pt heater strips；The sensitive material is a kind of mixture, including
SnO2/MnO2Composite hollow ball and Ni nano-powders.
2. gas sensor according to claim 1, it is characterised in that：The SnO2/MnO2Composite hollow ball is with carbonaceous
Polysaccharide microsphere is template, prepared by hydro-thermal method, the SnO2/MnO2The particle diameter of composite hollow ball is 150nm, SnO2With MnO2Matter
Amount is than being 3:2.
3. gas sensor according to claim 1, it is characterised in that：The sensitive material operating temperature is 200 DEG C.
4. gas sensor according to claim 2, it is characterised in that：The Ni nano-powders and SnO2/MnO2Compound air
The mass ratio of bulbus cordis is 1:9.
5. gas sensor according to claim 4, it is characterised in that：The particle diameter of the Ni nano-powders is 500nm.
6. gas sensor according to claim 1, it is characterised in that：Between the sensitive material and earthenware also
Provided with one layer of tin film, the tin film is prepared on the earthenware using the method for cold spraying.
7. gas sensor according to claim 6, it is characterised in that：The tin film thickness is 500 μm.
8. gas sensor according to claim 1, it is characterised in that：The preparation process of the gas sensor is：
Step 1, prepare carbonaceous polysaccharide microsphere：
5g glucose is dissolved in into 35ml to go in example water to form settled solution, then put it into water heating kettle, by the water heating kettle
10h is kept at 190 DEG C, by the precursor liquid ethanol of gained and goes example water to clean repeatedly 5 times, dries 13h at 80 DEG C afterwards,
Obtain carbonaceous polysaccharide microsphere；
Step 2, prepare SnO2/MnO2Composite hollow ball：
By 0.2mmol MnCl2·4H2O is dissolved in the solution A that 0.02mol/L is formed in 10ml dimethylformamide；Will
0.4mmol SnCl4·5H2O is dissolved in the solution B that 0.04mol/L is formed in 10ml dimethylformamide；0.3g carbonaceous is more
Sugared microballoon ultrasound, which is dissolved in 50ml dimethylformamide, forms solution C；Then solution A, B are slowly dropped in solution C, together
When continuous magnetic agitation；Then after ultrasonic 30min, mixed solution is placed at room temperature 1 day, then with ethanol and deionized water
Alternating centrifugal is cleaned, and solid mixture is dried into 10h at 70 DEG C；
Step 3, prepare sensitive material：
Ni nano-powders are mixed with the solid mixture after above-mentioned centrifugal drying, ground uniformly, then by its high-temperature calcination；
Step 4, prepare gas sensor：
The surface cold spraying tin film between two gold electrodes being parallel to each other of earthenware, then by the production after above-mentioned high-temperature calcination
Thing is coated onto tin film surface, thickness is 500 μm, is done under infrared lamp with going example water to be well mixed and forming starchiness
After dry 30min, the earthenware is placed in 400 DEG C of sintering 2h in Muffle furnace, then Pt heater strips are inserted into earthenware, to
The operating temperature of sensor is provided, the gas sensor is obtained after welding lead.
9. gas sensor according to claim 8, it is characterised in that：In the step 3, high-temperature burning process is：Point
4h is calcined not at 240 DEG C, calcines 5h at 510 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116574507A (en) * | 2023-04-27 | 2023-08-11 | 广州大学 | Hollow manganese dioxide/carbon dot composite material and preparation method and application thereof |
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| CN116574507B (en) * | 2023-04-27 | 2024-04-16 | 广州大学 | Hollow manganese dioxide/carbon dot composite material and preparation method and application thereof |
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Effective date of registration: 20180611 Address after: 101309 No. 1, Qianlong Road, Jung Zhuang village, Mu Lin Town, Shunyi District, Beijing. Applicant after: An Wei Address before: No. 33, Guilin Luan Road, Guilin, the Guangxi Zhuang Autonomous Region Applicant before: Zhong Yongsong |
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Application publication date: 20180406 |