CN108562615B - Nitrogen dioxide leakage detection device working at room temperature - Google Patents
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Abstract
The invention relates to a nitrogen dioxide leakage detection device working at room temperature, which comprises a nitrogen dioxide gas sensor, a temperature detection module, a signal amplification module, a digital-to-analog converter, a microprocessor,Monitoring a display and an audible and visual alarm; the nitrogen dioxide gas sensor is of a thick film type, a ceramic substrate is used as a substrate, a finger inserting electrode is arranged on the ceramic substrate, a sensitive film is arranged on the finger inserting electrode, and the sensitive film is a CuO nano rod and Al/In2O3Mixtures of/RGO composites.
Description
Technical Field
The invention relates to the field of gas leakage detection, in particular to a nitrogen dioxide leakage detection device working at room temperature.
Background
For a large amount of nitrogen dioxide leakage, the nitrogen dioxide has pungent smell, is easy to be found and can take corresponding measures in time; however, if a slight amount of leakage occurs without detection means, the leakage is not easily detected, and thus, personnel and property damage is easily caused.
Disclosure of Invention
The invention aims to provide a nitrogen dioxide leakage detection device working at room temperature to solve the problems.
The embodiment of the invention provides a nitrogen dioxide leakage detection device working at room temperature, which comprises a nitrogen dioxide gas sensor, a temperature detection module, a signal amplification module, a digital-to-analog converter, a microprocessor, a monitoring display and an audible and visual alarm, wherein the nitrogen dioxide gas sensor is connected with the temperature detection module; the nitrogen dioxide gas sensor is used for sensing the concentration of leaked nitrogen dioxide, the output end of the nitrogen dioxide gas sensor is connected with the signal amplification module, the temperature detection module is used for sensing the ambient temperature, the output end of the temperature detection module is connected with the digital-to-analog converter, the output end of the signal amplification module is connected with the digital-to-analog converter, the output end of the digital-to-analog converter is connected with the microprocessor, and the microprocessor is connected with the detection display and the audible and visual alarm; the nitrogen dioxide gas sensor is of a thick film type, a ceramic substrate is used as a substrate, a finger inserting electrode is arranged on the ceramic substrate, a sensitive film is arranged on the finger inserting electrode, and the sensitive film is a CuO nano rod and Al/In2O3Mixtures of/RGO composites.
The technical scheme provided by the embodiment of the invention can have the following beneficial effects:
1. the sensitive materials of the nitrogen dioxide sensor are CuO nano-rods and Al/In2O3The mixture of the/RGO composite material has the advantages of high sensitivity and short response time at room temperature;
2. the leakage condition is automatically detected, the concentration is displayed in real time, and when the leakage concentration reaches the maximum allowable value, an alarm signal is immediately sent out so that maintenance personnel can conveniently enter an emergency processing state and adopt corresponding safety protection measures.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention. It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention, as claimed.
Drawings
The invention is further illustrated by means of the attached drawings, but the embodiments in the drawings do not constitute any limitation to the invention, and for a person skilled in the art, other drawings can be obtained on the basis of the following drawings without inventive effort.
Fig. 1 is a schematic block diagram of the circuit of the present invention.
Detailed Description
Reference will now be made in detail to the exemplary embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, like numbers in different drawings represent the same or similar elements unless otherwise indicated. The embodiments described in the following exemplary embodiments do not represent all embodiments consistent with the present invention. Rather, they are merely examples of apparatus and methods consistent with certain aspects of the invention, as detailed in the appended claims.
The embodiment of the invention relates to a nitrogen dioxide leakage detection device working at room temperature, which comprises a nitrogen dioxide gas sensor, a temperature detection module, a signal amplification module, a digital-to-analog converter, a microprocessor, a monitoring display and an audible and visual alarm.
The nitrogen dioxide gas sensor is used for sensing the concentration of leaked nitrogen dioxide, the output end of the nitrogen dioxide gas sensor is connected with the signal amplification module, the temperature detection module is used for sensing the ambient temperature, the output end of the temperature detection module is connected with the digital-to-analog converter, the output end of the signal amplification module is connected with the digital-to-analog converter, the output end of the digital-to-analog converter is connected with the microprocessor, and the microprocessor is connected with the detection display and the audible and visual alarm.
When the device is used, the nitrogen dioxide gas sensor is placed at a position where gas is easy to leak, a sensor signal is processed through the signal amplification module and the digital-to-analog converter, the microprocessor collects a concentration signal and an environment temperature signal of the processed gas sensor, displays concentration data and temperature data, and drives the sound-light alarm device to alarm when the concentration reaches a warning line.
In a specific embodiment, the nitrogen dioxide gas sensor is based on a graphene composite material, and the sensor has good sensitivity and fast response recovery time at room temperature. The nitrogen dioxide gas sensor is of a thick film type, a ceramic substrate is used as a substrate, a finger inserting electrode is arranged on the ceramic substrate, a sensitive film is arranged on the finger inserting electrode, the thickness of the sensitive film is 0.2mm, and the sensitive film is a CuO nano rod and Al/In2O3Mixtures of/RGO composites.
The main sources of nitrogen dioxide are industrial fuel high-temperature combustion, motor vehicle exhaust emission, nitric acid nitrogen fertilizer and the like. It is a common toxic and harmful gas, NO2Performance of sensor for monitoring NO in environment2Has great significance. At present, for NO2The research of the gas sensor mainly focuses on the materials such as metal oxide semiconductor, solid electrolyte and the like, wherein the sensitive materials of the metal oxide semiconductor type sensor mainly comprise WO3、SnO2、ZnO、In2O3However, the above materials need to operate at a higher temperature, increase the internal consumption of the sensor, and cause inconvenience in miniaturization and integration of the sensor, and further, the selectivity and stability thereof need to be improved. As mentioned above, NO based on conventional metal oxides2The sensor needs to work at higher temperature, the internal consumption of the sensor is increased, and NO based on the graphene material2The sensor is expected to operate at room temperature. Graphene is a novel carbon material, has both semiconductor and metal properties due to its special atomic structure and complex energy band structure, and has excellent electron transfer properties, and is widely used for developing room-temperature NO2SensingA device. However, the adsorption of gas molecules is limited due to the existence of dangling bonds on the surface of graphene, such as hydroxyl, carboxyl, epoxy and the like, and NO is based on pure graphene materials2The sensor has the defects of poor gas selectivity, low sensitivity, long response recovery time and the like, and the NO of the graphene can be obviously improved after the graphene is doped2The sensitivity of (2). At present, the traditional gas sensitive materials such as noble metals, metal oxides, conducting polymers and the like are utilized to modify graphene and the ternary compound formed by the noble metals, the metal oxides, the conducting polymers and the like is generally applied to improving the graphene-based NO2The sensing performance of the sensor is improved by adopting the method, not only enabling each component to exert the advantage of sensitivity to gas, but also adjusting the physical and chemical properties of the graphene-based material. Graphene composite materials have been widely used for research of gas sensors, but graphene-based NO at room temperature2The sensor still has the problems of poor selectivity, low sensitivity, long response recovery time and the like.
In the technical scheme of the invention, the sensitive materials are CuO nano rods and Al/In2O3The combination of the mixture of the/RGO composite material and the RGO composite material can produce unexpected technical effects on the sensitive material, so that the sensitivity of the sensor is greatly improved: specifically, In the sensitive material of the present invention, Al/In is added2O3coating/RGO dispersion liquid drops on the surface of the CuO nano rod so as to form the sensor sensitive material; the CuO nano rod forms a first-level sensitive material, and the Al/In2O3the/RGO composite material forms a secondary sensitive material, the RGO is In a lamellar layer, and Al and In2O3Is nano particles, is modified on the surface of the lamella RGO, and further, the lamella RGO is adsorbed on the surface of the CuO nano rod, and the CuO nano rod forms the Al/In2O3Natural dispersing mechanism of/RGO composite material, so that Al/In2O3/RGO composite materials with NO2The contact area is greatly increased, and the sensitivity of the sensor is improved; in addition, In terms of composition, Reduced Graphene Oxide (RGO) is mixed with CuO nanorods and In2O3Al is combined, and the semiconductor performance of the graphene is regulated and controlled by doping the graphene, so that the graphite can be obviously improvedAlkenyl NO2The sensitivity characteristics of the sensor; the above binding pair NO2The method plays a sensitive role, improves the transmission rate of electrons in the sensitive material and produces unexpected technical effects.
Preferably, In the sensitive material, the CuO nanorods and Al/In2O3The mass ratio of the/RGO composite material is 5: 1. In the technical scheme of the invention, the sensitive material generates unexpected technical effect by further controlling the mass ratio and the doping amount, so that the sensitivity performance of the sensor is greatly improved.
The CuO nanorod is prepared by a hydrothermal method, and has the diameter of 60nm and the length of 500 nm. Copper oxide is a p-type narrow-band-gap semiconductor material, and the nano copper oxide material has the unusual characteristics of light, electricity, magnetism, catalysis and the like, and has application in the aspects of catalysts, battery cathode materials, photo-thermal and light guide materials and the like; according to the technical scheme, the copper oxide nanorod is combined with the graphene, the semiconductor performance of the graphene is regulated, unexpected technical effects are generated, and the sensing performance of the sensitive material is improved. The Al/In2O3the/RGO composite material is prepared by a hydrothermal method, and the composite material has a two-dimensional sheet structure, Al and In2O3Are all nano particles which are uniformly loaded on the surface of RGO; the grain diameter of the Al nano particles is 20 nm; said In2O3The particle size of the nano particles is 10 nm; in the composite material, Al and In2O3And RGO in a mass ratio of 2:3: 2. In the composite material, Al and In are doped on the surface of graphene2O3The nano particles provide more active sites, the electron transmission rate of the sensitive material is improved, the composite material has a porous structure, and meanwhile, pn junctions are formed between the nano particles and graphene, so that the sensitive characteristic is improved.
The preparation process of the nitrogen dioxide gas sensor comprises the following steps:
s1: first, 40ml of a NaOH solution having a concentration of 1.5mol/L was prepared, and 0.4mmol of Cu (NO) was added thereto3)2·3H2O powder, stirring to dissolveAdding 3mmol of hexadecyl trimethyl ammonium bromide, stirring at 50 ℃ for 60min, changing the solution from blue to black, transferring the obtained suspension into a polytetrafluoroethylene reaction kettle with the volume of 50ml, reacting at 150 ℃ for 24h, naturally cooling to room temperature, performing centrifugal separation, washing the precipitate with deionized water and ethanol for several times, and drying the precipitate in a vacuum drying oven for 12h to obtain CuO nanorod powder;
s2, preparation of Al/In2O3/RGO composite material
a) Preparation of graphite oxide
The preparation of GO is accomplished by a modified Hummers process:
firstly, 0.1g of graphite powder and 2.3ml of concentrated sulfuric acid solution are mixed and stirred for 24 hours at room temperature, then 10mg of sodium nitrate is added into the mixture and stirred for 40 minutes, then the mixture is placed into an ice bath, 0.3g of potassium permanganate is slowly added into the mixture, after the mixture is uniformly stirred, the mixture is heated in a water bath at 35-40 ℃ for 40 minutes until the reaction is viscous, 4.6ml of distilled water is slowly added, the mixture is heated and stirred for 15 minutes at 75 ℃, and finally, 14ml of distilled water and 1ml of hydrogen peroxide solution are added into the mixture to stop the reaction; then, repeatedly washing the obtained mixture with distilled water until the solution is neutral, separating graphite powder deposited at the bottom of the solution and not stripped by oxidation from GO sheets dispersed in the aqueous solution by stripping by oxidation, and re-dispersing the dried GO in deionized water to prepare a GO solution with the concentration of 1.0 mg/ml;
b) 1ml of the above GO solution was added to 40ml of distilled water, and then InCl was added3·4H2Adding O into GO dispersion liquid, performing ultrasonic dispersion for 30min, transferring the solution into a 50ml hydrothermal reaction kettle, sealing, placing the kettle In an oven for reaction at 180 ℃ for 12h, and performing centrifugal separation on the obtained product to obtain In2O3an/RGO dispersion; adding 0.4M Al (NO)3)3Adding the solution and 1% sodium acetate solution into the In2O3Heating the mixed solution to 100 ℃ In the/RGO dispersion liquid for reaction for 60min, and centrifugally separating and washing the obtained product to obtain the Al/In2O3/RGO composite materialA material dispersion;
s3, plasma treatment
Al/In obtained above2O3Coating dispersed liquid drops of the/RGO composite material on the surface of CuO nanorod powder, grinding for 30min, performing ultrasonic treatment for 15min to uniformly mix the powder, and then performing low-temperature radio frequency argon plasma treatment on the mixture, wherein the plasma generation device is in an inductive coupling type, the working frequency is 12.67MHz, the power is 350W, the air pressure is 50Pa, the gas flow rate is 18sccm, and the treatment time is 50 min;
in the technical scheme of the invention, Al/In is mixed2O3The dispersed liquid drops of the/RGO composite material are coated on the surface of the CuO nanorod powder, the graphene sheet layer can be effectively adsorbed on the surface of the copper oxide nanorod, the specific surface area is further increased, in addition, the surface property of the composite material can be effectively improved and the surface activity is increased after the mixture is subjected to argon plasma treatment, and the improvement of NO is realized2The sensitivity and the lowest detection concentration are reduced, and unexpected technical effects are generated;
then, uniformly mixing the mixture after the plasma treatment with a proper amount of water for removing the sample, grinding the mixture in a mortar for 10min, coating the obtained paste on the surface of a ceramic substrate with an interdigital electrode, and drying to obtain the nitrogen dioxide gas sensor; specifically, the finger inserting electrode is a Pt electrode, the width of a Pt electrode line is 0.12mm, the distance between fingers is 0.15mm, and the thickness of the finger inserting electrode is 0.1-0.2 mm.
Comparative example 1
Compared with the above embodiment, no CuO nanorod is arranged in the sensitive film.
Comparative example 2
In contrast to the above examples, the Al/In of the sensitive film2O3The Al nanoparticles are not arranged in the/RGO composite material.
Comparative example 3
In contrast to the above examples, the Al/In of the sensitive film2O3In is not provided In the/RGO composite material2O3Nanoparticles.
Comparative example 4
In contrast to the above examples, the sensitive film was not plasma treated.
NO of the invention by using gas-sensitive characteristic tester2And (3) testing the sensor: firstly, injecting target gas with certain concentration into a sealed test cavity, and then, after the target gas is uniformly mixed with air in the cavity, adding NO2The sensor is placed in the test chamber.
NO in the invention2The sensitivity of the sensor, response recovery time, etc. are defined conventionally in the art.
First, the sensors obtained in examples and comparative examples were each used for 5ppm of NO at room temperature2Response tests were performed with the following results:
it can be seen that the sensor obtained by the embodiment has obvious advantages in sensitivity and response recovery time, and unexpected technical effects are produced.
Then, the sensor obtained in example was used for 1ppm of NO2Response testing was performed and found to be 13.6 in sensitivity, reducing NO2The lowest detected concentration of (c).
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, but rather as the subject matter of the invention is to be construed in all aspects and as broadly as possible, and all changes, equivalents and modifications that fall within the true spirit and scope of the invention are therefore intended to be embraced therein.
Claims (2)
1. A nitrogen dioxide leakage detection device working at room temperature is characterized by comprising a nitrogen dioxide gas sensor, a temperature detection module, a signal amplification module, a digital-to-analog converter, a microprocessor, a monitoring display and an audible and visual alarm;
the nitrogen dioxide gas sensor is used for sensing the concentration of leaked nitrogen dioxide, the output end of the nitrogen dioxide gas sensor is connected with the signal amplification module, the temperature detection module is used for sensing the ambient temperature, the output end of the temperature detection module is connected with the digital-to-analog converter, the output end of the signal amplification module is connected with the digital-to-analog converter, the output end of the digital-to-analog converter is connected with the microprocessor, and the microprocessor is connected with the detection display and the audible and visual alarm;
the nitrogen dioxide gas sensor is of a thick film type, a ceramic substrate is used as a substrate, a finger inserting electrode is arranged on the ceramic substrate, a sensitive film is arranged on the finger inserting electrode, and the sensitive film is a CuO nano rod and Al/In2O3Mixtures of/RGO composites;
the thickness of the sensitive film is 0.2 mm;
the sensitive film is formed by mixing Al/In2O3the/RGO dispersed liquid drop is coated on the surface of the CuO nano rod, so as to form the sensitive film of the sensor, the RGO is In a sheet layer, and Al and In2O3Is nano particles and is modified on the surface of the sheet layer RGO;
the CuO nanorod is prepared by a hydrothermal method, and has the diameter of 60nm and the length of 500 nm;
the CuO nanorod and the Al/In2O3The mass ratio of the/RGO composite material is 5: 1;
the Al/In2O3the/RGO composite material is prepared by a hydrothermal method, and the composite material has a two-dimensional sheet structure, Al and In2O3Are all nano particles which are uniformly loaded on the surface of RGO; the grain diameter of the Al nano particles is 20 nm; said In2O3The particle size of the nano particles is 10 nm; in the composite material, Al and In2O3And RGO in a mass ratio of 2:3: 2.
2. The nitrogen dioxide leakage detection device working at room temperature according to claim 1, wherein the nitrogen dioxide gas sensor is prepared by the following steps:
s1: first, 40ml of a NaOH solution having a concentration of 1.5mol/L was prepared, and 0.4mmol of Cu (NO) was added thereto3)2·3H2O powder, stirring well to dissolve, adding 3mmol cetyl trimethyl ammonium bromide, stirring at 50 deg.C for 60min to turn the solution from blue to black, transferring the obtained suspension into a polytetrafluoroethylene reaction kettle with volume of 50mlReacting at 150 ℃ for 24h, naturally cooling to room temperature, centrifugally separating, washing the precipitate with deionized water and ethanol for several times, and drying the precipitate in a vacuum drying oven for 12h to obtain CuO nanorod powder;
s2, preparation of Al/In2O3/RGO composite material
a) The preparation of GO is accomplished by a modified Hummers process: firstly, 0.1g of graphite powder and 2.3ml of concentrated sulfuric acid solution are mixed and stirred for 24 hours at room temperature, then 10mg of sodium nitrate is added into the mixture and stirred for 40 minutes, then the mixture is placed into an ice bath, 0.3g of potassium permanganate is slowly added into the mixture, after the mixture is uniformly stirred, the mixture is heated in a water bath at 35-40 ℃ for 40 minutes until the reaction is viscous, 4.6ml of distilled water is slowly added, the mixture is heated and stirred for 15 minutes at 75 ℃, and finally, 14ml of distilled water and 1ml of hydrogen peroxide solution are added into the mixture to stop the reaction; then, repeatedly washing the obtained mixture with distilled water until the solution is neutral, separating graphite powder deposited at the bottom of the solution and not stripped by oxidation from GO sheets dispersed in the aqueous solution by stripping by oxidation, and re-dispersing the dried GO in deionized water to prepare a GO solution with the concentration of 1.0 mg/ml; b) 1ml of the above GO solution was added to 40ml of distilled water, and then InCl was added3·4H2Adding O into GO dispersion liquid, performing ultrasonic dispersion for 30min, transferring the solution into a 50ml hydrothermal reaction kettle, sealing, placing the kettle In an oven for reaction at 180 ℃ for 12h, and performing centrifugal separation on the obtained product to obtain In2O3an/RGO dispersion; adding 0.4M Al (NO)3)3Adding the solution and 1% sodium acetate solution into the In2O3Heating the mixed solution to 100 ℃ In the/RGO dispersion liquid for reaction for 60min, and centrifugally separating and washing the obtained product to obtain the Al/In2O3an/RGO composite dispersion;
s3, plasma treatment
Al/In obtained above2O3Coating dispersed liquid drops of the/RGO composite material on the surface of CuO nano-rod powder, grinding for 30min, carrying out ultrasonic treatment for 15min to uniformly mix the CuO nano-rod powder and the RGO composite material, and then carrying out low-temperature treatment on the mixturePerforming radio frequency argon plasma treatment, wherein a plasma generating device is in an inductive coupling type, the working frequency is 12.67MHz, the power is 350W, the air pressure is 50Pa, the gas flow rate is 18sccm, and the treatment time is 50 min;
then, uniformly mixing the mixture after the plasma treatment with a proper amount of water for removing the sample, grinding the mixture in a mortar for 10min, coating the obtained paste on the surface of a ceramic substrate with an interdigital electrode, and drying to obtain the nitrogen dioxide gas sensor; the finger inserting electrode is a Pt electrode, the width of a Pt electrode line is 0.12mm, the distance between fingers is 0.15mm, and the thickness of the finger inserting electrode is 0.1-0.2 mm.
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