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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- 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 28
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000001514 detection method Methods 0.000 title claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000000725 suspension Substances 0.000 claims abstract description 25
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims description 30
- 238000000608 laser ablation Methods 0.000 claims description 22
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- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 15
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 9
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
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- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
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- 229910021529 ammonia Inorganic materials 0.000 description 1
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- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
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- 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
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Abstract
本发明属于传感器制备技术领域，尤其涉及一种气敏传感器及在二氧化氮气体检测的应用。本发明提供了一种气敏传感器，所述气敏传感器设有表面滴加白碳悬浮液后干燥的叉指电极。本发明还提供了上述气敏传感器在二氧化氮气体检测的应用。经检测可得，本发明提供的技术方案制得的气敏传感器，在常温可见光下，即可对不同浓度的二氧化氮进行检测，具有响应性好、灵敏度高、响应及恢复时间快、重现性好、选择性强、抗湿性好的优点；且制备简单，生产成本低，绿色环保，尤其适用于环境中低浓度二氧化氮的检测。本发明提供的一种气敏传感器及其在二氧化氮气体检测的应用，解决了现有技术中，气敏传感器需在高温或紫外光下才可工作的技术缺陷。
The invention belongs to the technical field of sensor preparation, in particular to a gas sensor and its application in nitrogen dioxide gas detection. The invention provides a gas sensor, which is provided with interdigital electrodes which are dried after dripping white carbon suspension on the surface. The present invention also provides the application of the above gas sensor in nitrogen dioxide gas detection. After testing, it can be seen that the gas sensor prepared by the technical solution provided by the present invention can detect nitrogen dioxide with different concentrations under visible light at room temperature, and has good responsiveness, high sensitivity, fast response and recovery time, and high reliability. The invention has the advantages of good presentability, strong selectivity, and good moisture resistance; and the preparation is simple, the production cost is low, and the method is green and environmentally friendly, and is especially suitable for the detection of low-concentration nitrogen dioxide in the environment. The invention provides a gas sensor and its application in nitrogen dioxide gas detection, which solves the technical defect in the prior art that the gas sensor needs to work under high temperature or ultraviolet light.
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)
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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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