CN108562615A - A kind of nitrogen dioxide leakage detector of working and room temperature - Google Patents
A kind of nitrogen dioxide leakage detector of working and room temperature Download PDFInfo
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- CN108562615A CN108562615A CN201810002106.3A CN201810002106A CN108562615A CN 108562615 A CN108562615 A CN 108562615A CN 201810002106 A CN201810002106 A CN 201810002106A CN 108562615 A CN108562615 A CN 108562615A
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- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 title claims abstract description 47
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 title claims abstract description 35
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000002131 composite material Substances 0.000 claims abstract description 29
- 239000007789 gas Substances 0.000 claims abstract description 28
- 239000000203 mixture Substances 0.000 claims abstract description 21
- 239000010409 thin film Substances 0.000 claims abstract description 13
- 239000000758 substrate Substances 0.000 claims abstract description 12
- 239000000919 ceramic Substances 0.000 claims abstract description 10
- 230000003321 amplification Effects 0.000 claims abstract description 9
- 238000003199 nucleic acid amplification method Methods 0.000 claims abstract description 9
- 239000010408 film Substances 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 14
- 239000002105 nanoparticle Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 239000006185 dispersion Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000001514 detection method Methods 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 241000446313 Lamella Species 0.000 claims description 5
- 239000002270 dispersing agent Substances 0.000 claims description 5
- 239000002073 nanorod Substances 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 238000003851 corona treatment Methods 0.000 claims description 4
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 2
- 230000008878 coupling Effects 0.000 claims description 2
- 238000010168 coupling process Methods 0.000 claims description 2
- 238000005859 coupling reaction Methods 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000008236 heating water Substances 0.000 claims description 2
- 229960002163 hydrogen peroxide Drugs 0.000 claims description 2
- 230000001939 inductive effect Effects 0.000 claims description 2
- 239000004570 mortar (masonry) Substances 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000012286 potassium permanganate Substances 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 239000001632 sodium acetate Substances 0.000 claims description 2
- 235000017281 sodium acetate Nutrition 0.000 claims description 2
- 239000004317 sodium nitrate Substances 0.000 claims description 2
- 235000010344 sodium nitrate Nutrition 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
- 239000000725 suspension Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims 3
- 239000007864 aqueous solution Substances 0.000 claims 1
- 238000000527 sonication Methods 0.000 claims 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical group [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 35
- 239000000463 material Substances 0.000 description 19
- 229910021389 graphene Inorganic materials 0.000 description 16
- 230000035945 sensitivity Effects 0.000 description 9
- 230000000694 effects Effects 0.000 description 6
- 230000004044 response Effects 0.000 description 6
- 238000011084 recovery Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 229960004643 cupric oxide Drugs 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- IWLUJCZGMDWKRT-UHFFFAOYSA-N azane oxygen(2-) titanium(4+) Chemical compound N.[O-2].[Ti+4].[O-2] IWLUJCZGMDWKRT-UHFFFAOYSA-N 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000000618 nitrogen fertilizer Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000000505 pernicious effect Effects 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000011540 sensing material Substances 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The present invention relates to a kind of nitrogen dioxide leakage detectors of working and room temperature, including nitrogen dioxide gas sensor, temperature detecting module, signal amplification module, digital analog converter, microprocessor, monitor display and audible-visual annunciator；The nitrogen dioxide gas sensor is thick-film type, uses ceramic substrate for substrate, is equipped on the ceramic substrate and inserts finger electrode, and the slotting electrode that refers to is equipped with sensitive thin film, and the sensitive thin film is CuO nanometer rods and Al/In2O3The mixture of/RGO composite materials.
Description
Technical field
The present invention relates to a kind of nitrogen dioxide leak detection of Leakage inspection field more particularly to working and room temperature dresses
It sets.
Background technology
Larger amount of nitrogen dioxide is leaked, since nitrogen dioxide has penetrating odor, be easy to be found and can and
When take appropriate measures；But in case of micro leakage, while there is no detection means, this leakage is not easy to be found,
To be easy to cause personnel and property loss.
Invention content
The present invention is intended to provide a kind of nitrogen dioxide leakage detector of working and room temperature, set forth above to solve the problems, such as.
A kind of nitrogen dioxide leakage detector of working and room temperature, including nitrogen dioxide are provided in the embodiment of the present invention
Gas sensor, temperature detecting module, signal amplification module, digital analog converter, microprocessor, monitor display and sound-light alarm
Device；Content of nitrogen dioxide of the nitrogen dioxide gas sensor for sensitive leakage, output end and signal amplification module phase
Even, temperature detecting module is used for sensitive environment temperature, and output end is connected with digital analog converter, the signal amplification module it is defeated
Outlet is connected with digital analog converter, and the output end of the digital analog converter is connected with microprocessor, and microprocessor is shown with detection
Device is connected with audible-visual annunciator；The nitrogen dioxide gas sensor is thick-film type, uses ceramic substrate for substrate, in the ceramics
Substrate, which is equipped with to insert, refers to electrode, inserts finger electrode and is equipped with sensitive thin film, the sensitive thin film is CuO nanometer rods and Al/In2O3/
The mixture of RGO composite materials.
The technical solution that the embodiment of the present invention provides can include the following benefits：
1, the sensitive material of nitrogen dioxide sensor of the present invention is CuO nanometer rods and Al/In2O3/ RGO composite materials mix
Object is closed, has the advantages that high sensitivity, response time are short at room temperature；
2, automatic Leakage Detection situation, real-time display concentration send out alarm immediately when leakage concentration reaches maximum permissible value
Signal, so that maintenance personnel enters emergent management state, using corresponding safety precautions.
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
Obviously, or practice through the invention is recognized.It should be understood that above general description and following detailed description are only
It is exemplary and explanatory, the present invention can not be limited.
Description of the drawings
Using attached drawing, the invention will be further described, but the embodiment in attached drawing does not constitute any limit to the present invention
System, for those of ordinary skill in the art, without creative efforts, can also obtain according to the following drawings
Other attached drawings.
Fig. 1 is the schematic block circuit diagram of the present invention.
Specific implementation mode
Example embodiments are described in detail here, and the example is illustrated in the accompanying drawings.Following description is related to
When attached drawing, unless otherwise indicated, the same numbers in different drawings indicate the same or similar elements.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 device and method of some aspects being described in detail in claims, of the invention.
The embodiment of the present invention is related to a kind of nitrogen dioxide leakage detector of working and room temperature, including nitrogen dioxide gas
Sensor, temperature detecting module, signal amplification module, digital analog converter, microprocessor, monitor display and audible-visual annunciator.
Content of nitrogen dioxide of the nitrogen dioxide gas sensor for sensitive leakage, output end amplify mould with signal
Block is connected, and temperature detecting module is used for sensitive environment temperature, and output end is connected with digital analog converter, the signal amplification module
Output end be connected with digital analog converter, the output end of the digital analog converter is connected with microprocessor, microprocessor with detection
Display is connected with audible-visual annunciator.
In use, nitrogen dioxide gas sensor is placed on the position that gas easily leaks, sensor signal is put by signal
Big module and digital analog converter processing, the gas sensor concentration signal and ambient temperature signal that microprocessor acquisition process is crossed,
And show concentration data and temperature data, when concentration reaches warning line, driving acoustic-optic alarm alarm.
In a kind of specific embodiment, which is based on graphene composite material, the sensor
Operating temperature at room temperature, has good sensitivity and faster response recovery time.The nitrogen dioxide gas sensor is
Thick-film type uses ceramic substrate for substrate, is equipped on the ceramic substrate and inserts finger electrode, inserts finger electrode and is equipped with sensitive thin film,
The sensitive thin film thickness is 0.2mm, and the sensitive thin film is CuO nanometer rods and Al/In2O3The mixture of/RGO composite materials.
Nitrogen dioxide main source is industrial fuel high-temp combustion, automotive emission, nitric acid nitrogenous fertilizer etc..It is a kind of
It common are poison, pernicious gas, NO2The performance of sensor is for the NO in monitoring of environmental2It is significant.Currently, for NO2Gas
The research of body sensor is concentrated mainly on the materials such as metal-oxide semiconductor (MOS), solid electrolyte, wherein metal oxide is partly led
The sensitive material of body formula sensor includes mainly WO3、SnO2、ZnO、In2O3Deng however, above-mentioned material is needed in higher temperature
Lower work, increases the in-fighting of sensor, also, for sensor miniaturization, it is integrated make troubles, in addition, its selectivity and
Stability still needs to improve.As described above, the NO based on INVENTIONConventional metal-oxide2Sensor needs to work at a higher temperature,
Increase sensor in-fighting, and the NO based on grapheme material2Sensor is expected to realize and work at room temperature.Graphene is a kind of
Novel carbon material, since the band structure of its special atomic structure and complexity makes it while having characteristic of semiconductor and metal
Characteristic, and there is excellent electron transmission performance, it is widely used in developing room temperature NO2Sensor.But due to graphene surface
There are dangling bonds, such as hydroxyl, carboxyl, epoxy group, limit the absorption of gas molecule, the NO based on pure state grapheme material2
Sensor sheet reveals the shortcomings of poor to gas-selectively, sensitivity is low, response recovery time is long, and by being adulterated to graphene
Afterwards, graphene can be obviously improved to NO2Sensitivity.Currently, using traditional gas sensitive, such as the oxidation of noble metal, metal
Object, conducting polymer etc. are grapheme modified and form ternary complex by them and are widely used in and improve graphene-based NO2
The sensing capabilities of sensor can not only make each ingredient play the advantage to gas sensitization, and can adjust using the above method
The physicochemical properties of arthrolith mertenyl material are to improve sensing capabilities.Graphene composite material has been widely used for gas biography
The research of sensor, but graphene-based NO at room temperature2There are still poor selectivity, low, the response recovery time length of sensitivity etc. for sensor
Problem.
In technical solution of the present invention, the sensitive material is CuO nanometer rods and Al/In2O3The mixing of/RGO composite materials
Object, the two combines so that the sensitive material produces unexpected technique effect so that the sensitive performance of sensor substantially carries
It is high：Specifically, it is by Al/In in the above-mentioned sensitive material of the present invention2O3/ RGO dispersant liquid drops are coated onto CuO nanorod surfaces, from
And form the sensor sensing material；The CuO nanometers of bar construction level-one sensitive material, the Al/In2O3/ RGO composite materials
Two level sensitive material is constituted, RGO is in lamella, Al and In2O3For nano-particle, modify on the surfaces lamella RGO, in turn, lamella RGO
CuO nanorod surfaces are adsorbed on, which constitutes the Al/In2O3The natural dispersive mechanism of/RGO composite materials, makes
Obtain the Al/In2O3/ RGO composite materials and NO2Contact area greatly increases, and improves transducer sensitivity；In addition, in ingredient
Aspect, redox graphene (RGO) and CuO nanometer rods, In2O3, Al combine, by doped graphene, regulate and control the half of graphene
Conductor performance can be obviously improved graphene-based NO2The sensitivity characteristic of sensor；Above-mentioned combination is to NO2Sensitization is played, is carried
The transmission rate of electronics, produces unexpected technique effect in high sensitive material.
Preferably, in above-mentioned sensitive material, the CuO nanometer rods and Al/In2O3The mass ratio of/RGO composite materials is
5:1.In technical solution of the present invention, further by controlling quality when doping so that the sensitive material produces expectation not
The technique effect arrived so that the sensitive performance of sensor greatly improves.
The CuO nanometer rods are prepared by hydro-thermal method, a diameter of 60nm of the CuO nanometer rods, length 500nm.
Copper oxide is a kind of p-type narrow bandgap semiconductor material, and nano oxidized copper product has uncommon light, electricity, magnetic and catalysis etc. special
Property, there is application in catalyst, cell negative electrode material, photo-thermal and light-guide material etc.；In technical solution of the present invention, pass through
Cupric oxide nano-rod is combined with graphene, regulates and controls the semiconducting behavior of graphene, unexpected technique effect is produced, carries
The high sensing capabilities of sensitive material.The Al/In2O3/ RGO composite materials are prepared by hydro-thermal method, which is in
Two-dimensional sheet structure, Al and In2O3It is nano-particle, is uniformly supported on the surfaces RGO；The Al nano particle diameters are
20nm；The In2O3Nano particle diameter is 10nm；In the composite material, Al, In2O3Mass ratio with RGO is 2:3:2.
In the composite material, by adulterating Al and In on the surface of graphene2O3Nano-particle provides more active sites, improves
The electron transfer rate of sensitive material so that composite material has porous structure, meanwhile, shape between nano-particle and graphene
At pn-junction, to improve sensitivity characteristic.
The preparation process of nitrogen dioxide gas sensor of the present invention is：
S1：First, configuration concentration is the NaOH solution 40ml of 1.5mol/L, and the Cu (NO of 0.4mmol are added thereto3)2·
3H2O powder, stirs evenly, and makes it dissolve, and the cetyl trimethylammonium bromide of 3mmol is then added, is stirred at 50 DEG C
60min, solution become black from blue, gained suspension are transferred in the ptfe autoclave that volume is 50ml,
It reacts for 24 hours, cooled to room temperature, centrifuges at 150 DEG C, spend example water and ethyl alcohol washing precipitation for several times, then will sink
The dry 12h in vacuum drying chamber that forms sediment obtains CuO nanometer rods powder；
S2 prepares Al/In2O3/ RGO composite materials
A) graphite oxide is prepared
The preparation of GO is completed by improved Hummers methods：
First, the graphite powder of 0.1g is mixed with the concentrated sulfuric acid solution of 2.3ml, is stirred at room temperature for 24 hours, it then, will
The sodium nitrate of 10mg be added in mixture continue stir 40min then mixture is placed in ice bath, thereto slowly plus
Enter 0.3g potassium permanganate, after object to be mixed stirs evenly, 35-40 DEG C of heating water bath processing 40min is carried out to it, until reaction is viscous
It is thick, be slow added into 4.6ml distilled water, and by said mixture at 75 DEG C heating stirring 15min, finally, into mixture
The hydrogenperoxide steam generator of 14ml distilled water and 1ml is added to terminate reaction；Then, gained mixture is repeatedly clear with distilled water
It washes, until solution is in neutrality, then water is dispersed in by the graphite powder for being deposited on the not oxidized stripping in solution bottom and by oxidation stripping
GO piece layer separations in solution, the GO after drying is dispersed in again be configured in example water a concentration of 1.0mg/ml GO it is molten
Liquid；
B) the above-mentioned GO solution of 1ml is added in 40ml distilled water, then by InCl3·4H2O is added to the dispersion liquid of GO
In, solution is then transferred in the hydrothermal reaction kettle of 50ml by ultrasonic disperse 30min, and 180 DEG C of reactions in an oven are put after sealing
12h centrifuges products therefrom, obtains In2O3/ RGO dispersion liquids；Again by the Al (NO of 0.4M3)3Solution and mass fraction are
1% sodium acetate solution is added to above-mentioned In2O3In/RGO dispersion liquids, mixed solution is heated to 100 DEG C of reaction 60min, gained
Product is centrifuged, washs, and obtains the Al/In2O3/ RGO composite material dispersion liquids；
S3, corona treatment
By Al/In obtained above2O3/ RGO composite material dispersant liquid drops are coated onto CuO nanometer rods powder surface, grinding
30min, be ultrasonically treated 15min, make its be uniformly mixed, then, by mixture carry out low temperature radio frequency argon plasma processing, wait from
Sub- generating means is inductive coupling, and working frequency 12.67MHz, power 350W, air pressure 50Pa, gas flow rate is
18sccm, processing time 50min；
In technical solution of the present invention, by Al/In2O3/ RGO composite material dispersant liquid drops are coated onto CuO nanometer rods powder surface,
The graphene sheet layer can effectively be adsorbed on cupric oxide nano-rod surface, further increase specific surface area, in addition, mixture passes through
Argon plasma processing is crossed, the surface nature of composite material can be effectively improved, increases surface-active, for improving NO2It is sensitive
Degree, reduction minimal detectable concentration produce unexpected technique effect；
Then, by after corona treatment mixture with go example water to be uniformly mixed in right amount, ground in mortar
Gained paste is coated on the ceramic bases surface for inserting finger electrode, after dry, obtains the titanium dioxide nitrogen by 10min
Body sensor；Specifically, the slotting finger electrode is Pt electrodes, Pt electrode line width is 0.12mm, and it is 0.15mm to refer to spacing, is inserted
Finger thickness of electrode is 0.1~0.2mm.
Reference examples 1
Compared to above-described embodiment, CuO nanometer rods are not provided in the sensitive thin film.
Reference examples 2
Compared to above-described embodiment, the Al/In of the sensitive thin film2O3It is not provided with Al nano-particles in/RGO composite materials.
Reference examples 3
Compared to above-described embodiment, the Al/In of the sensitive thin film2O3It is not provided with In in/RGO composite materials2O3Nanoparticle
Son.
Reference examples 4
Compared to above-described embodiment, the sensitive thin film does not pass through plasma treatment.
Using gas-sensitive property tester to NO of the present invention2Sensor is tested：First certain density object gas is noted
Enter into sealing test chamber, wait for air in object gas and chamber after mixing, then by NO2Sensor is put into test chamber.
NO in the present invention2Sensitivity, response recovery time of sensor etc. use this field usual definition.
First, the sensor obtained respectively to embodiment and reference examples is at room temperature to the NO of 5ppm2Response test is carried out,
Test result is as follows table：
It can be seen that the sensor that embodiment obtains all has clear superiority in sensitivity, response recovery time, produces
Unexpected technique effect.
Then, by sensor obtained by embodiment to the NO of 1ppm2Response test is carried out, it is found that sensitivity is 13.6, reduces
NO2Minimal detectable concentration.
The foregoing is merely the preferred modes of the present invention, are not intended to limit the invention, all spirit and original in the present invention
Within then, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (7)
1. a kind of nitrogen dioxide leakage detector of working and room temperature, which is characterized in that including nitrogen dioxide gas sensor, temperature
Spend detection module, signal amplification module, digital analog converter, microprocessor, monitor display and audible-visual annunciator；
Content of nitrogen dioxide of the nitrogen dioxide gas sensor for sensitive leakage, output end and signal amplification module phase
Even, temperature detecting module is used for sensitive environment temperature, and output end is connected with digital analog converter, the signal amplification module it is defeated
Outlet is connected with digital analog converter, and the output end of the digital analog converter is connected with microprocessor, and microprocessor is shown with detection
Device is connected with audible-visual annunciator；
The nitrogen dioxide gas sensor is thick-film type, uses ceramic substrate for substrate, is equipped on the ceramic substrate and inserts finger
Electrode is inserted and refers to electrode equipped with sensitive thin film, and the sensitive thin film is CuO nanometer rods and Al/In2O3/ RGO composite materials mix
Close object.
2. a kind of nitrogen dioxide leakage detector of working and room temperature according to claim 1, which is characterized in that described quick
Sense film thickness is 0.2mm.
3. a kind of nitrogen dioxide leakage detector of working and room temperature according to claim 1, which is characterized in that described quick
It is by Al/In to feel film2O3/ RGO dispersant liquid drops are coated onto CuO nanorod surfaces, to form the sensor sensing film,
The RGO is in lamella, Al and In2O3For nano-particle, modify on the surfaces lamella RGO.
4. a kind of nitrogen dioxide leakage detector of working and room temperature according to claim 3, which is characterized in that described
CuO nanometer rods are prepared by hydro-thermal method, a diameter of 60nm of the CuO nanometer rods, length 500nm.
5. a kind of nitrogen dioxide leakage detector of working and room temperature according to claim 3, which is characterized in that described
CuO nanometer rods and Al/In2O3The mass ratio of/RGO composite materials is 5:1.
6. a kind of nitrogen dioxide leakage detector of working and room temperature according to claim 3, which is characterized in that described
Al/In2O3/ RGO composite materials are prepared by hydro-thermal method, which is in two-dimensional sheet structure, Al and In2O3It is
Nano-particle is uniformly supported on the surfaces RGO；The Al nano particle diameters are 20nm；The In2O3Nano particle diameter is
10nm；In the composite material, Al, In2O3Mass ratio with RGO is 2:3:2.
7. a kind of nitrogen dioxide leakage detector of working and room temperature according to claim 3, which is characterized in that described two
The preparation process of nitrogen oxide gas sensor is：
S1：First, configuration concentration is the NaOH solution 40ml of 1.5mol/L, and the Cu (NO of 0.4mmol are added thereto3)2·3H2O
Powder stirs evenly, and makes it dissolve, and the cetyl trimethylammonium bromide of 3mmol is then added, 60min is stirred at 50 DEG C,
Solution becomes black from blue, gained suspension is transferred in the ptfe autoclave that volume is 50ml, at 150 DEG C
For 24 hours, cooled to room temperature centrifuges for reaction, spends example water and ethyl alcohol washing precipitation for several times, then will be deposited in vacuum
Dry 12h obtains CuO nanometer rods powder in drying box；
S2 prepares Al/In2O3/ RGO composite materials
A) preparation of GO is completed by improved Hummers methods：First, by the concentrated sulfuric acid of the graphite powder of 0.1g and 2.3ml
Solution mixes, and is stirred at room temperature for 24 hours, then, the sodium nitrate of 10mg is added in mixture and continues to stir 40min, then,
Mixture is placed in ice bath, is slowly added to 0.3g potassium permanganate thereto, after object to be mixed stirs evenly, 35- is carried out to it
40 DEG C of heating water bath processing 40min is slow added into 4.6ml distilled water, and by said mixture at 75 DEG C until reacting sticky
The hydrogenperoxide steam generator of 14ml distilled water and 1ml are finally added into mixture to terminate reaction by lower heating stirring 15min；So
Afterwards, repeatedly wash with distilled water by gained mixture, until solution is in neutrality, then the not oxidized stripping in solution bottom will be deposited on
Graphite powder and the GO piece layer separations by oxidation stripping dispersion in aqueous solution, example water is dispersed in by the GO after drying again
In be configured to the GO solution of a concentration of 1.0mg/ml；B) the above-mentioned GO solution of 1ml is added in 40ml distilled water, then will
InCl3·4H2O is added in the dispersion liquid of GO, and solution is then transferred to the hydrothermal reaction kettle of 50ml by ultrasonic disperse 30min
In, 180 DEG C of reaction 12h in an oven are put after sealing, and products therefrom is centrifuged, In is obtained2O3/ RGO dispersion liquids；Again will
Al (the NO of 0.4M3)3The sodium acetate solution that solution and mass fraction are 1% is added to above-mentioned In2O3In/RGO dispersion liquids, it will mix
It closes solution and is heated to 100 DEG C of reaction 60min, products therefrom is centrifuged, washs, and obtains the Al/In2O3/ RGO composite woods
Expect dispersion liquid；
S3, corona treatment
By Al/In obtained above2O3/ RGO composite material dispersant liquid drops are coated onto CuO nanometer rods powder surface, grinding 30min, surpass
Sonication 15min makes it be uniformly mixed, and then, mixture is carried out the processing of low temperature radio frequency argon plasma, plasma fills
It is set to inductive coupling, working frequency 12.67MHz, power 350W, air pressure 50Pa, gas flow rate 18sccm, when processing
Between be 50min；
Then, by after corona treatment mixture with go example water to be uniformly mixed in right amount, 10min is ground in mortar, will
Gained paste is coated on the ceramic bases surface for inserting finger electrode, after dry, obtains the nitrogen dioxide gas sensor；
The slotting finger electrode is Pt electrodes, and Pt electrode line width is 0.12mm, and it is 0.15mm to refer to spacing, and it is 0.1 to insert finger thickness of electrode
~0.2mm.
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