CN110927218A - Preparation method of gas-sensitive material for detecting nitrogen dioxide and gas sensor - Google Patents
Preparation method of gas-sensitive material for detecting nitrogen dioxide and gas sensor Download PDFInfo
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Abstract
The invention provides a preparation method of a gas-sensitive material for detecting nitrogen dioxide and a gas sensor, wherein the preparation method comprises the following steps: weighing carboxylated carbon nanotubes and adding a solvent to form a first mixed solution; adding a dispersing agent into the first mixed solution, and performing ultrasonic dispersion treatment to form a second mixed solution; carrying out centrifugal sedimentation on the second mixed solution, wherein the upper layer liquid after the centrifugal sedimentation treatment is the gas-sensitive material; wherein the dispersant comprises sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, triton and polyvinyl pyrrolidone. In the preparation method of the gas sensitive material for detecting nitrogen dioxide, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, triton and polyethylene pyrrolidone are added as dispersing agents, so that the problem of dispersibility of the gas sensitive material is well solved, and the test performance of the gas sensitive material can be improved.
Description
Technical Field
The invention relates to the technical field of sensors, in particular to a preparation method of a gas sensitive material for detecting nitrogen dioxide and a gas sensor for detecting nitrogen dioxide.
Background
As a novel material, the nano material has wide application. However, the nano material is easy to agglomerate, so that the application range of the nano material is limited, and the nano material solution is required to have better dispersibility in some applications.
Common dispersing methods for nano materials include the following methods:
1. an electric dispersion method: since the isoelectric point exists on the surface of the nanoparticles, the dispersion stability of the nanoparticles can be increased when the pH difference between the isoelectric points is maximized by adjusting the pH, but this method is only suitable for dispersion in water.
2. Chemical dispersion method: namely, the nanoparticles are surface-modified with a coupling agent, a surfactant, a dispersant, etc., to improve the dispersibility of the nanoparticles.
3. Physical dispersion method: the dispersion of the nanomaterial is achieved by high-speed stirring using a high-speed shear disperser, grinding dispersion using a three-roll mill or a grinder, or ball milling using a ball mill or ultrasonic dispersion.
The chemical dispersion method is a method which is applied in many cases because the chemical dispersion method has the most stable dispersion effect relatively. However, a certain amount of surfactant is added in the chemical dispersion method, so that the service performance of the nano material in some application fields is limited, and therefore, it is very important to find a dispersing agent which can solve the problem of the dispersibility of the nano material and does not influence the performance of the nano material.
Disclosure of Invention
The invention aims to provide a preparation method of a gas-sensitive material for detecting nitrogen dioxide, in the preparation method, a proper dispersing agent is added, so that the problem of dispersity of the gas-sensitive material can be solved, the testing performance of the gas-sensitive material is not influenced, and the application field of the gas-sensitive material is greatly improved.
In particular, the invention provides a preparation method of a gas-sensitive material for detecting nitrogen dioxide, which comprises the following steps:
weighing carboxylated carbon nanotubes and adding a solvent to form a first mixed solution;
adding a dispersing agent into the first mixed solution, and performing ultrasonic dispersion treatment to form a second mixed solution;
carrying out centrifugal sedimentation on the second mixed solution, wherein the upper layer liquid after the centrifugal sedimentation treatment is the gas-sensitive material;
wherein the dispersant comprises sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, triton and polyvinyl pyrrolidone.
Further, in the step of forming the first mixed solution, the mass of the carboxylated carbon nanotube is weighed to be 1mg-10mg, and the amount of the added solvent is 1ml-10 ml.
Further, the solvent is one or more of deionized water, DMF and ethanol.
Further, the dispersant accounts for 2-50% of the mass of the carboxylated carbon nanotube.
Further, in the dispersing agent, the sodium dodecyl benzene sulfonate accounts for 2-20% of the mass of the carboxylated carbon nanotube, the sodium dodecyl sulfate accounts for 2-25% of the mass of the carboxylated carbon nanotube, the triton accounts for 2-5% of the mass of the carboxylated carbon nanotube, and the polyvinylpyrrolidone accounts for 1-2% of the mass of the carboxylated carbon nanotube.
Further, in the step of forming the second mixed liquid, the time of ultrasonic dispersion is 10min to 60 min.
Further, in the step of performing centrifugal sedimentation on the second mixed solution, the centrifugal speed is 5000-10000 rmp.
The present invention also provides a gas sensor for detecting nitrogen dioxide, comprising:
a substrate;
at least two electrodes arranged on the surface of the substrate;
the gas-sensitive material prepared by the preparation method in the embodiment is dripped on the surface of the substrate and covers at least two electrodes so as to be packaged into the gas sensor after aging treatment.
Further, the substrate is one of a PCB substrate, a ceramic substrate, a silicon substrate and a PET substrate.
In the preparation method of the gas sensitive material for detecting nitrogen dioxide, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, triton and polyethylene pyrrolidone are added as dispersing agents, so that the problem of dispersibility of the gas sensitive material is well solved, and the test performance of the gas sensitive material can be improved.
The above and other objects, advantages and features of the present invention will become more apparent to those skilled in the art from the following detailed description of specific embodiments thereof, taken in conjunction with the accompanying drawings.
Drawings
Some specific embodiments of the invention will be described in detail hereinafter, by way of illustration and not limitation, with reference to the accompanying drawings. The same reference numbers in the drawings identify the same or similar elements or components. Those skilled in the art will appreciate that the drawings are not necessarily drawn to scale. In the drawings:
fig. 1 is a flowchart of a method of preparing a gas sensitive material for detecting nitrogen dioxide according to an embodiment of the present invention;
FIG. 2 is a graph of the response of a gas sensor of the present invention to nitrogen dioxide without the addition of a dispersant;
FIG. 3 is a graph of the response of a dispersant-loaded gas sensor of the present invention to nitrogen dioxide;
figure 4 is a graph of the response of six gas sensors of the present invention with dispersant added to the nitrogen dioxide.
Detailed Description
The preparation method of the gas-sensitive material for detecting nitrogen dioxide provided by the embodiment of the invention comprises the following steps:
s1, weighing the carboxylated carbon nanotubes, and adding a solvent to form a first mixed solution;
s2, adding a dispersing agent into the first mixed solution, and carrying out ultrasonic dispersion treatment to form a second mixed solution;
and S3, performing centrifugal sedimentation on the second mixed solution, wherein the upper layer liquid after the centrifugal sedimentation is a gas-sensitive material.
Wherein the dispersant comprises sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, triton (the component of the triton is polyoxyethylene-8-octyl phenyl ether) and polyvinyl pyrrolidone.
Specifically, referring to fig. 1, in the method for preparing a gas-sensitive material for detecting nitrogen dioxide according to an embodiment of the present invention, firstly, carboxylated carbon nanotubes may be weighed, and the carboxylated carbon nanotubes may have better dispersibility than pure carbon nanotubes. And adding a solvent into the carboxylated carbon nanotube, and performing oscillation or ultrasonic treatment to obtain a first mixed solution. Then, a dispersant, which may be sodium dodecylbenzene sulfonate, sodium lauryl sulfate, triton, and polyvinyl pyrrolidone, is added to the first mixed solution. After the dispersing agent is added, the cell crusher can be used for carrying out ultrasonic dispersion treatment on the cell, and a second mixed solution can be obtained after the dispersion treatment. And finally, performing centrifugal sedimentation on the second mixed solution by using a centrifugal machine, and after the centrifugal sedimentation treatment, reserving the upper layer liquid to obtain the gas sensitive material prepared by the invention.
According to the preparation method, the gas-sensitive material for detecting nitrogen dioxide can be prepared only by adding the solvent and the dispersing agent according to a normal preparation process, carrying out ultrasonic dispersion and then carrying out centrifugal treatment. In the preparation method of the gas sensitive material for detecting nitrogen dioxide, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, triton and polyvinyl pyrrolidone are added as dispersing agents, so that the problem of dispersibility of the gas sensitive material is well solved, namely the problem of consistency of zero point resistance of a gas sensor is solved, and meanwhile, the test performance of the gas sensitive material can be improved. In the preparation method of the invention, the response sensitivity of the nitrogen oxide (such as nitrogen dioxide) is effectively improved by adding the dispersant.
In some embodiments of the present invention, the amount of the solvent is 1ml to 10ml, and the amount of the carboxylated carbon nanotube is 1mg to 10 mg. The solvent may be one or more of deionized water, DMF and ethanol. The addition amount of the dispersant can be 2-50% of the mass percent of the carboxylated carbon nanotube. Preferably, in the dispersant, the mass percent of sodium dodecyl benzene sulfonate in the carboxylated carbon nanotubes is 2-20%, the mass percent of sodium dodecyl sulfate in the carboxylated carbon nanotubes is 2-25%, the mass percent of triton in the carboxylated carbon nanotubes is 2-5%, and the mass percent of polyvinylpyrrolidone in the carboxylated carbon nanotubes is 1-2%.
In some embodiments of the present invention, in the step of forming the second mixed liquid, the time of the ultrasonic dispersion is 10min to 60 min. And in the step of carrying out centrifugal sedimentation on the second mixed solution, the centrifugal speed is 5000-10000 rmp.
The gas-sensitive material prepared by the preparation method is packaged into a sensor, and the performance of the gas-sensitive material is tested, see fig. 2 to fig. 4, wherein fig. 2 is a response curve graph of the gas sensor without the dispersant of the invention on nitrogen dioxide, and as can be seen from fig. 2, the gas-sensitive material obtained without the dispersant tests five concentrations of 0.1ppm, 0.2ppm, 0.5ppm, 0.8ppm and 1ppm after being packaged into the gas sensor, the response is gradually increased along with the increase of the concentration of the nitrogen dioxide gas, and the gas-sensitive material has a concentration gradient, wherein the response value corresponding to the 1ppm of the nitrogen dioxide gas is approximately 8%. Fig. 3 is a graph showing the response curve of the gas sensor with the dispersant added to nitrogen dioxide, under the same test conditions as fig. 2, when the gas sensor packaged with the gas sensitive material prepared with the dispersant added is tested for the response of nitrogen dioxide, five concentrations of 0.1ppm, 0.2ppm, 0.5ppm, 0.8ppm and 1ppm are also tested, and the response value gradually increases with the increase of the concentration of nitrogen dioxide, and the concentration gradient exists. The gas sensor added with the dispersing agent tests that the response value of 1ppm of nitrogen dioxide gas reaches 60 percent. Compared to fig. 2, the test response value increased nearly 8-fold over the gas sensor without the dispersant at the same nitrogen dioxide concentration. That is to say, the gas sensitive material for detecting nitrogen dioxide prepared by the invention can improve the test performance of the gas sensitive material. Fig. 4 is a graph showing the response of six gas sensors added with a dispersant to nitrogen dioxide, and fig. 4 shows the test performance of six gas sensors packaged with the gas-sensitive material prepared by the preparation method of the present invention, and it can be seen from fig. 4 that the consistency of the gas sensors for testing nitrogen dioxide gas is very good.
In summary, in the preparation method of the gas sensitive material for detecting nitrogen dioxide, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, triton and polyvinyl pyrrolidone are added as dispersing agents, so that the problem of dispersibility of the gas sensitive material is well solved, and the test performance of the gas sensitive material can be improved.
The invention also provides a gas sensor for detecting nitrogen dioxide, which mainly comprises a substrate, at least two electrodes and a gas-sensitive material. The gas sensitive material prepared by the preparation method of the embodiment is coated on the surface of the substrate with the electrodes and covers the electrodes, the gas sensitive material is coated on the substrate with the electrodes and then subjected to aging treatment, and resistance test before encapsulation can be performed after the aging treatment. And finally, packaging the substrate coated with the gas sensitive material after the aging treatment to form the gas sensor. The substrate may adopt one of a PCB substrate, a ceramic substrate, a silicon substrate and a PET substrate. Of course, other configurations and operating principles of the gas sensor of the present application will be understood and readily implemented by those skilled in the art, and will not be described in detail.
The gas sensitive material prepared by the preparation method of the embodiment of the invention is packaged into a sensor, and the performance of the gas sensitive material is tested, referring to fig. 2 to fig. 4, wherein fig. 2 is a response curve graph of the gas sensor without the dispersant of the invention on nitrogen dioxide, and as can be seen from fig. 2, the gas sensitive material without the dispersant tests five concentrations of 0.1ppm, 0.2ppm, 0.5ppm, 0.8ppm and 1ppm after being packaged into the gas sensor, the response is gradually increased along with the increase of the concentration of the nitrogen dioxide gas, and the gas sensitive material has a concentration gradient, wherein the response value corresponding to 1ppm of the nitrogen dioxide gas is approximately 8%. Fig. 3 is a graph showing the response curve of the gas sensor with the dispersant added to nitrogen dioxide, under the same test conditions as fig. 2, when the gas sensor packaged with the gas sensitive material prepared with the dispersant added is tested for the response of nitrogen dioxide, five concentrations of 0.1ppm, 0.2ppm, 0.5ppm, 0.8ppm and 1ppm are also tested, and the response value gradually increases with the increase of the concentration of nitrogen dioxide, and the concentration gradient exists. The gas sensor added with the dispersing agent tests that the response value of 1ppm of nitrogen dioxide gas reaches 60 percent. Compared to fig. 2, the test response value increased nearly 8-fold over the gas sensor without the dispersant at the same nitrogen dioxide concentration. That is to say, the gas sensitive material for detecting nitrogen dioxide prepared by the invention can improve the test performance of the gas sensitive material. Fig. 4 is a graph showing the response of six gas sensors with dispersant added to nitrogen dioxide, and fig. 4 shows the test performance of six gas sensors packaged by the gas sensitive material prepared by the preparation method of the present invention, and it can be seen from fig. 4 that the consistency of the gas sensors for testing nitrogen dioxide gas is very good.
Thus, it should be appreciated by those skilled in the art that while a number of exemplary embodiments of the invention have been illustrated and described in detail herein, many other variations or modifications consistent with the principles of the invention may be directly determined or derived from the disclosure of the present invention without departing from the spirit and scope of the invention. Accordingly, the scope of the invention should be understood and interpreted to cover all such other variations or modifications.
Claims (9)
1. A preparation method of a gas-sensitive material for detecting nitrogen dioxide is characterized by comprising the following steps:
weighing carboxylated carbon nanotubes and adding a solvent to form a first mixed solution;
adding a dispersing agent into the first mixed solution, and performing ultrasonic dispersion treatment to form a second mixed solution;
carrying out centrifugal sedimentation on the second mixed solution, wherein the upper layer liquid after the centrifugal sedimentation treatment is the gas-sensitive material;
wherein the dispersant comprises sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, triton and polyvinyl pyrrolidone.
2. The method according to claim 1, wherein in the step of forming the first mixed solution, the carboxylated carbon nanotubes are weighed to have a mass of 1mg to 10mg, and the solvent is added in an amount of 1ml to 10 ml.
3. The method for preparing a gas-sensitive material for detecting nitrogen dioxide as claimed in claim 1, wherein the solvent is one or more of deionized water, DMF and ethanol.
4. The method for preparing the gas-sensitive material for detecting nitrogen dioxide as claimed in claim 1, wherein the dispersant accounts for 2-50% by mass of the carboxylated carbon nanotubes.
5. The method according to claim 1, wherein in the dispersant, the sodium dodecyl benzene sulfonate accounts for 2-20% by mass of the carboxylated carbon nanotubes, the sodium dodecyl sulfate accounts for 2-25% by mass of the carboxylated carbon nanotubes, the triton accounts for 2-5% by mass of the carboxylated carbon nanotubes, and the polyvinylpyrrolidone accounts for 1-2% by mass of the carboxylated carbon nanotubes.
6. The method for preparing a gas-sensitive material for detecting nitrogen dioxide as claimed in claim 1, wherein in the step of forming the second mixed liquid, the time for ultrasonic dispersion is 10min to 60 min.
7. The method for preparing a gas-sensitive material for detecting nitrogen dioxide as claimed in claim 1, wherein the step of subjecting the second mixed solution to centrifugal sedimentation has a centrifugal speed of 5000 to 10000 rmp.
8. A gas sensor for detecting nitrogen dioxide, comprising:
a substrate;
at least two electrodes arranged on the surface of the substrate;
the gas-sensitive material prepared by the preparation method according to any one of claims 1 to 7, which is coated on the surface of the substrate and covers at least two of the electrodes to be packaged into the gas sensor after an aging treatment.
9. The gas sensor for detecting nitrogen dioxide as claimed in claim 8, wherein the substrate is one of a PCB substrate, a ceramic substrate, a silicon substrate, and a PET substrate.
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| CN111413374A (en) * | 2020-04-20 | 2020-07-14 | 苏州慧闻纳米科技有限公司 | Preparation method of gas-sensitive material for detecting hydrogen sulfide at room temperature and gas sensing chip |
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