CN111351818B - Gas sensor and application thereof in nitrogen dioxide gas detection - Google Patents
Gas sensor and application thereof in nitrogen dioxide gas detection Download PDFInfo
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- CN111351818B CN111351818B CN202010316080.7A CN202010316080A CN111351818B CN 111351818 B CN111351818 B CN 111351818B CN 202010316080 A CN202010316080 A CN 202010316080A CN 111351818 B CN111351818 B CN 111351818B
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Abstract
The invention belongs to the technical field of sensor preparation, and particularly relates to a gas sensor and application thereof in nitrogen dioxide gas detection. The invention provides a gas sensor which is provided with an interdigital electrode, wherein the interdigital electrode is dried after white carbon suspension is dripped on the surface of the interdigital electrode. The invention also provides application of the gas sensor in nitrogen dioxide gas detection. The gas sensor prepared by the technical scheme provided by the invention can detect nitrogen dioxide with different concentrations under normal-temperature visible light, and has the advantages of good responsiveness, high sensitivity, quick response and recovery time, good reproducibility, strong selectivity and good moisture resistance; and the method is simple to prepare, low in production cost, green and environment-friendly, and is particularly suitable for detecting low-concentration nitrogen dioxide in the environment. The gas sensor and the application thereof in nitrogen dioxide gas detection provided by the invention solve the technical defect that the gas sensor can work only under high temperature or ultraviolet light in the prior art.
Description
Technical Field
The invention belongs to the technical field of sensor preparation, and particularly relates to a gas sensor and application thereof in nitrogen dioxide gas detection.
Background
With the development of industrialization, more and more toxic and harmful gases are generated, and the gas sensor is more and more paid attention as a device for detecting the toxic and harmful gases.
In the prior art, gas sensor materials all need to work under high temperature or ultraviolet light, the high temperature can have the problem of safety when in use, and the ultraviolet light also has the problem of harm to human bodies, thereby bringing limitation to the application of the gas sensor.
In view of the above, the present invention provides a gas sensor and an application thereof in nitrogen dioxide detection, which are used to solve the technical defect that the gas sensor needs to work under high temperature or ultraviolet light in the prior art, and thus the problem to be solved by the technical staff in the art is urgently needed.
Disclosure of Invention
In view of this, the present invention provides a gas sensor and an application thereof in nitrogen dioxide detection, which are used to solve the technical defect that the gas sensor can only work at high temperature or ultraviolet light in the prior art.
The invention provides a gas sensor which is provided with an interdigital electrode, wherein the interdigital electrode is dried after white carbon suspension is dripped on the surface of the interdigital electrode.
Preferably, the concentration of the white carbon suspension is 1-2 mg/ml, and the dropping amount of the white carbon suspension is 0.2～0.4ml/cm2。
Preferably, the substrate of the interdigital electrode is a silicon-silicon dioxide substrate, and the silicon-silicon dioxide substrate is subjected to a dropwise adding step after being pretreated and purified.
Preferably, the pretreatment method is that the silicon-silica substrate is dried in vacuum after being ultrasonically cleaned using any one or more of toluene, acetone, absolute ethanol and distilled water.
Preferably, the time of ultrasonic cleaning is 5-10 min/time, and the frequency of ultrasonic cleaning is 3-5 times.
Preferably, the preparation method of the white carbon suspension comprises the following steps:
s1, soaking the target material in absolute ethyl alcohol, and in a protective atmosphere, focusing a laser beam on the surface of the target material to perform a pulse laser ablation reaction after the laser beam sequentially passes through a total reflection lens and a focusing lens;
s2, after the pulse laser ablation reaction is finished, dripping the solution of the reaction system on a substrate, and evaporating the solvent to dryness to obtain white carbon;
and S3, mixing the white carbon with deionized water to obtain a white carbon suspension.
Preferably, in S1, the target material is a gold target material, the diameter of a focused laser beam spot is 0.1cm, and the protective atmosphere is nitrogen and/or argon.
Preferably, in S1, the reaction time of the pulse laser ablation reaction is 10 to 30min, the laser frequency of the pulse laser ablation reaction is 1 to 10Hz, and the single pulse energy of the pulse laser ablation reaction is 100 to 800 mJ.
Preferably, in S2, the substrate is a silicon wafer or a glass sheet.
The invention also provides an application of the gas sensor in nitrogen dioxide gas detection.
In summary, the invention provides a gas sensor, which is provided with an interdigital electrode, the surface of which is dried after white carbon suspension is dripped on the interdigital electrode. The invention also provides application of the gas sensor in nitrogen dioxide gas detection. The gas sensor prepared by the technical scheme provided by the invention can detect nitrogen dioxide with different concentrations under normal-temperature visible light, and has the advantages of good responsiveness, high sensitivity, quick response and recovery time, good reproducibility, strong selectivity and good moisture resistance; and the method is simple to prepare, low in production cost, green and environment-friendly, and is particularly suitable for detecting low-concentration nitrogen dioxide in the environment. The gas sensor and the application thereof in nitrogen dioxide gas detection provided by the invention solve the technical defect that the gas sensor can work only under high temperature or ultraviolet light in the prior art.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a UV-visible absorption spectrum of white carbon in a gas sensor;
FIG. 2 is an X-ray diffraction pattern of white carbon in a gas sensor;
FIG. 3 is a current-voltage curve of a gas sensor under room temperature visible light irradiation;
FIG. 4 is a resistance-time curve of a gas sensor under room temperature visible light irradiation conditions;
FIG. 5 is a response-concentration curve of a gas sensor to gases of different concentrations under room temperature visible light irradiation;
FIG. 6 is a graph of the long-term stability of a gas sensor to 50ppm nitrogen dioxide over a half year period under room temperature visible light irradiation;
FIG. 7 is a graph showing the selectivity of the gas sensor to 50ppm of different test gases under room temperature irradiation with visible light;
FIG. 8 shows the effect of humidity on a gas sensor under room temperature visible light irradiation.
Detailed Description
The invention provides a gas sensor and application thereof in nitrogen dioxide gas detection, which are used for solving the technical defect that the gas sensor can work only under high temperature or ultraviolet light in the prior art.
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to explain the present invention in more detail, the following describes a gas sensor and its application in nitrogen dioxide gas detection in detail with reference to the following embodiments.
Example 1
This example is a specific example of preparing a gas sensor product 1.
Preparation of white carbon suspension 1:
s1, soaking a gold target material with the purity of more than 99% in absolute ethyl alcohol, starting a laser erosion device in a nitrogen and/or argon protective atmosphere, focusing a laser beam on the surface of the target material to form a light spot with the diameter of 0.1cm after the laser beam sequentially passes through a total reflection lens and a focusing lens, carrying out pulse laser erosion reaction, forming a nanocrystal core on the solid target material under the action of high temperature and high pressure of laser, growing the nanocrystal core into nanoparticles in a liquid environment, cracking the absolute ethyl alcohol under the catalysis of the nanoparticles to generate isolated carbon atoms, and providing a nucleation thermodynamic environment for the isolated carbon atoms to form white carbon molecules under the action of the laser in a 2600-3800K high-temperature environment, so that the carbon atoms can spontaneously form white carbon and then gradually grow into the white carbon molecules; the reaction time of the pulse laser ablation reaction is 30min, the laser frequency of the pulse laser ablation reaction is 1-10 Hz, and the single pulse energy of the pulse laser ablation reaction is 100 mJ;
s2, after the pulse laser ablation reaction is finished, dripping the solution of the reaction system obtained in the step S1 on a silicon wafer substrate, and evaporating the solvent to dryness to obtain white carbon 1;
s3, 1mg of white carbon and 1ml of deionized water are mixed to obtain white carbon suspension 1.
Pretreatment and purification:the silicon-silicon dioxide substrate is pretreated and purified, and the specific purification method comprises the following steps: and ultrasonically cleaning the silicon-silicon dioxide substrate for 3-5 times by using any one or more of toluene, acetone, absolute ethyl alcohol and distilled water in sequence, and then drying in vacuum.
Interdigital electrode preparation: and dropwise adding the white carbon suspension 1 on the surface of the purified silicon-silicon dioxide substrate, volatilizing the solvent, and drying in vacuum to obtain the interdigital electrode 1. Wherein the dropping amount of the white carbon suspension 1 is 0.1ml/cm2。
The prepared interdigital electrode 1 is assembled to obtain the gas sensor product 1, and in the embodiment, the assembling step belongs to the prior art known by those skilled in the art, and details are not described herein.
Example 2
This example is a specific example of preparing a gas sensor product 2.
Preparation of white carbon suspension 2:
s1, soaking a gold target material with the purity of more than 99% in absolute ethyl alcohol, starting a laser erosion device in a nitrogen and/or argon protective atmosphere, focusing a laser beam on the surface of the target material to form a light spot with the diameter of 0.1cm after the laser beam sequentially passes through a total reflection lens and a focusing lens, carrying out pulse laser erosion reaction, forming a nanocrystal core on the solid target material under the action of high temperature and high pressure of laser, growing the nanocrystal core into nanoparticles in a liquid environment, cracking the absolute ethyl alcohol under the catalysis of the nanoparticles to generate isolated carbon atoms, and providing a nucleation thermodynamic environment for the isolated carbon atoms to form white carbon molecules under the action of the laser in a 2600-3800K high-temperature environment, so that the carbon atoms can spontaneously form white carbon and then gradually grow into the white carbon molecules; the reaction time of the pulse laser ablation reaction is 20min, the laser frequency of the pulse laser ablation reaction is 1-10 Hz, and the single pulse energy of the pulse laser ablation reaction is 800 mJ;
s2, after the pulse laser ablation reaction is finished, dripping the solution of the reaction system obtained in the step S1 on a glass sheet substrate, and evaporating the solvent to dryness to obtain white carbon 2;
s3, 2mg of white carbon and 1ml of deionized water are mixed to obtain white carbon suspension.
Pretreatment and purification:the silicon-silicon dioxide substrate is pretreated and purified, and the specific purification method comprises the following steps: and ultrasonically cleaning the silicon-silicon dioxide substrate for 3-5 times by using any one or more of toluene, acetone, absolute ethyl alcohol and distilled water in sequence, and then drying in vacuum.
Interdigital electrode preparation: and (3) after the white carbon suspension 2 is dripped on the surface of the purified silicon-silicon dioxide substrate, volatilizing the solvent and drying in vacuum to obtain the interdigital electrode 2. Wherein the dropping amount of the white carbon suspension 2 is 0.3ml/cm2。
The prepared interdigital electrode 2 is assembled to obtain the gas sensor product 2, and in the embodiment, the assembling step belongs to the prior art known by those skilled in the art, and is not described herein again.
Example 3
This example is a specific example of preparing a gas sensor product 3.
Preparation of white carbon suspension 3:
s1, soaking a gold target material with the purity of more than 99% in absolute ethyl alcohol, starting a laser erosion device in a nitrogen and/or argon protective atmosphere, focusing a laser beam on the surface of the target material to form a light spot with the diameter of 0.1cm after the laser beam sequentially passes through a total reflection lens and a focusing lens, carrying out pulse laser erosion reaction, forming a nanocrystal core on the solid target material under the action of high temperature and high pressure of laser, growing the nanocrystal core into nanoparticles in a liquid environment, cracking the absolute ethyl alcohol under the catalysis of the nanoparticles to generate isolated carbon atoms, and providing a nucleation thermodynamic environment for the isolated carbon atoms to form white carbon molecules under the action of the laser in a 2600-3800K high-temperature environment, so that the carbon atoms can spontaneously form white carbon and then gradually grow into the white carbon molecules; the reaction time of the pulse laser ablation reaction is 10min, the laser frequency of the pulse laser ablation reaction is 1-10 Hz, and the single pulse energy of the pulse laser ablation reaction is 600 mJ;
s2, after the pulse laser ablation reaction is finished, dripping the solution of the reaction system obtained in the step S1 on a silicon wafer substrate, and evaporating the solvent to dryness to obtain white carbon 3;
s3, 1.3mg white carbon and 1ml deionized water were mixed to obtain white carbon suspension 3.
Pretreatment and purification:the silicon-silicon dioxide substrate is pretreated and purified, and the specific purification method comprises the following steps: and ultrasonically cleaning the silicon-silicon dioxide substrate for 3-5 times by using any one or more of toluene, acetone, absolute ethyl alcohol and distilled water in sequence, and then drying in vacuum.
Interdigital electrode preparation: and dropwise adding the white carbon suspension 3 on the surface of the purified silicon-silicon dioxide substrate, volatilizing the solvent, and drying in vacuum to obtain the interdigital electrode 3. Wherein the dropping amount of the white carbon suspension 3 is 0.2ml/cm2。
The prepared interdigital electrode 3 is assembled to obtain the gas sensor product 3, and in the embodiment, the assembling step belongs to the prior art known by those skilled in the art, and is not described herein again.
Example 4
In this example, the white carbons 1 to 3 obtained in examples 1 to 3 were subjected to line scanning electron microscopy, transmission electron microscopy, X-ray diffraction, and ultraviolet-visible absorption spectroscopy.
The obtained white carbon molecule is rod-shaped, the length of the particle is 50 nm-100 nm and the width is 10 nm-30 nm, and the white carbon molecule is aggregated to form a flaky white carbon crystal.
Fig. 1 is a uv-vis absorption spectrum of white carbon, which can be observed and analyzed from fig. 1: the white carbon has two obvious absorption peaks at the wavelength of 230 nm and 238nm, and the ultraviolet visible absorption range of the white carbon is met.
FIG. 2 is the X-ray diffraction results of the sample, from which the analysis in FIG. 2 can be observed: the white carbon crystal obtained is a hexagonal crystal phase.
Example 5
This example is a specific example of the I-V performance test of the gas sensors 1 to 3 prepared in examples 1 to 3.
The test results obtained are further illustrated in fig. 3, from which it can be calculated that the gas sensor produced has a resistance of about 108 ohms at 4V, indicating that: the gas sensor prepared by the invention has higher resistance and is a good metal-semiconductor-metal sensor.
Example 6
This embodiment is a specific embodiment of the gas sensors 1 to 3 prepared in embodiments 1 to 3, which were subjected to a gas-sensitive test experiment.
The gas-sensitive test process is carried out at room temperature, the external atmospheric pressure and the nitrogen atmosphere, and the bias voltage of 7.4V is fixed between the two electrodes. The test uses JF02F gas-sensitive characterization system from agile technologies, inc, and the results obtained are shown in fig. 4 to 8.
It can be concluded from fig. 5 that the gas sensor has a good response to 2-50ppm nitrogen dioxide, the detection limit can reach 2ppm, and the response/recovery time is 100s and 90s, respectively. Description of the drawings: the prepared gas sensor has the advantages of good responsiveness, high sensitivity and quick response and recovery time.
As can be seen from fig. 4 and 6, the repeated responsiveness of the gas sensor to 50ppm nitrogen dioxide and the stability within half a year are substantially consistent, indicating that the stability of the gas sensor is good.
As can be seen from fig. 7, the gas sensor performs gas-sensitive tests on 50ppm of different gases including nitrogen dioxide, hydrogen, ammonia, propane, hydrogen sulfide, and methanol, and it can be seen that the white carbon material exhibits the maximum response to nitrogen dioxide among various test gases and has good selectivity to nitrogen dioxide.
As can be derived from fig. 8, humidity has less influence on the gas sensor.
In summary, the invention provides a gas sensor, which is provided with an interdigital electrode, the surface of which is dried after white carbon suspension is dripped on the interdigital electrode. The invention also provides application of the gas sensor in nitrogen dioxide gas detection. The gas sensor prepared by the technical scheme provided by the invention can detect nitrogen dioxide with different concentrations under normal-temperature visible light, and has the advantages of good responsiveness, high sensitivity, quick response and recovery time, good reproducibility, strong selectivity and good moisture resistance; and the method is simple to prepare, low in production cost, green and environment-friendly, and is particularly suitable for detecting low-concentration nitrogen dioxide in the environment. The gas sensor and the application thereof in nitrogen dioxide gas detection provided by the invention solve the technical defect that the gas sensor can work only under high temperature or ultraviolet light in the prior art.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A gas sensor applied to nitrogen dioxide gas detection is characterized in that the gas sensor is provided with an interdigital electrode, the surface of which is dried after white carbon suspension liquid is dripped;
the concentration of the white carbon suspension is 1-2 mg/ml, and the dropping amount of the white carbon suspension is 0.2-0.4 ml/cm2。
2. The gas sensor of claim 1, wherein the substrate of the interdigital electrode is a silicon-silicon dioxide substrate, and the silicon-silicon dioxide substrate is subjected to a dropping step after being purified by pretreatment.
3. The gas sensor of claim 2, wherein the pretreatment method is vacuum drying after the silicon-silica substrate is ultrasonically cleaned using any one or more solvents selected from the group consisting of toluene, acetone, absolute ethanol, and distilled water.
4. The gas sensor as claimed in claim 3, wherein the time of the ultrasonic cleaning is 5 to 10 min/time, and the number of times of the ultrasonic cleaning is 3 to 5 times.
5. The gas sensor of claim 1, wherein the white carbon suspension is prepared by:
s1, soaking the target material in absolute ethyl alcohol, and in a protective atmosphere, focusing a laser beam on the surface of the target material to perform a pulse laser ablation reaction after the laser beam sequentially passes through a total reflection lens and a focusing lens;
s2, after the pulse laser ablation reaction is finished, dripping the solution of the reaction system on a substrate, and evaporating the solvent to dryness to obtain white carbon;
and S3, mixing the white carbon with deionized water to obtain a white carbon suspension.
6. The gas sensor of claim 5, wherein in S1, the target is a gold target, the diameter of the focused laser beam spot is 0.1cm, and the protective atmosphere is nitrogen and/or argon.
7. The gas sensor according to claim 5, wherein in S1, the reaction time of the pulsed laser ablation reaction is 10-30 min, the laser frequency of the pulsed laser ablation reaction is 1-10 Hz, and the single pulse energy of the pulsed laser ablation reaction is 100-800 mJ.
8. The gas sensor of claim 5, wherein the substrate is a silicon wafer or a glass wafer in S2.
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| JP4245310B2 (en) * | 2001-08-30 | 2009-03-25 | 忠正 藤村 | Diamond suspension aqueous solution excellent in dispersion stability, metal film containing this diamond, and product thereof |
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