CN114873929B - Novel sensor material and preparation method thereof - Google Patents
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Abstract
The invention relates to a novel sensor material and a preparation method thereof, wherein the preparation method comprises the following steps: mixing and dissolving imidazole ionic liquid and pure water at room temperature to form ionic liquid aqueous solution, adding MXene material into the ionic liquid aqueous solution to obtain mixed solution, dropwise adding aniline ethanol solution into the mixed solution, carrying out reduced pressure rotary evaporation and concentration until the volume is less than one third of the original volume, coating the liquid in the bottle on a glass or ceramic substrate, then placing the glass or ceramic substrate in an oven for primary drying treatment, then carrying out atmospheric pressure plasma treatment, carrying out final drying treatment, taking out the glass or ceramic substrate and cooling the glass or ceramic substrate to room temperature, thus obtaining the modified imidazole ionic liquid. The method has the advantages that the ionic liquid and the oxidized polyaniline formed by in-situ polymerization are used for intercalation and surface modification of the two-dimensional MXene material, and the voltage-guided diffusion of the dielectric barrier discharge device and the polymerization-promoting diffusion of atmospheric pressure plasma are utilized, so that the sensing performance of the modified MXene material on NOx gas is remarkably improved, and the response value at room temperature is over 80.
Description
Technical Field
The invention belongs to the field of new materials, and particularly relates to a novel sensor material and a preparation method thereof.
Background
Nitrogen Oxides (NO) X ) Including a variety of compounds such as nitrous oxide, nitric oxide, nitrogen dioxide, dinitrogen trioxide, dinitrogen tetroxide, dinitrogen pentoxide, and the like. Besides nitrogen dioxide, other nitrogen oxides are extremely unstable and change into nitrogen dioxide and nitric oxide when exposed to light, moisture or heat, and nitric oxide changes into nitrogen dioxide again.
Research shows that the industrial waste gas emits trace NO to the environment X Can irritate the lung, causing respiratory diseases and lung cancer risk. For reducing NO X The harm to human health requires the development of effective means for ultra-low concentration NOx detection in the environment. The high selectivity and the low detection limit are key performance parameters of the gas sensor, and the traditional gas sensor is difficult to realize the ultra-low detection limit and the ultra-high selectivity at room temperature. How to design a gas-sensitive material for analyzing and detecting NOx with high sensitivity and high selectivity becomes a scientific problem to be solved urgently.
Disclosure of Invention
The invention aims to solve the technical problem of providing a novel sensor material and a preparation method thereof, and aims to overcome the defect that the sensitivity and selectivity of the existing gas sensitive material for detecting NOx are difficult to be considered.
The technical scheme for solving the technical problems is as follows: a preparation method of a novel sensor material comprises the following steps: mixing imidazole ionic liquid 1-butyl-3-methylimidazole ferric chloride salt and pure water at room temperature according to the weight ratio of 1:5-8, mixing and dissolving to form an ionic liquid aqueous solution, adding MXene material into the ionic liquid aqueous solution, and fully dispersing to obtain a mixed solution, wherein the dosage ratio of the MXene material to the 1-butyl-3-methylimidazole iron tetrachloride salt is 0.05-0.15g:1mL, dropwise adding an ethanol solution of aniline into the mixed solution at room temperature, and stirring, wherein the mass ratio of aniline to MXene in the mixed solution is (2-5): 1, stirring and reacting for 1-3h after finishing dripping, then decompressing, rotating, evaporating and concentrating until the liquid in the bottle is reduced to be less than one third of the original volume, coating the liquid in the bottle on a glass or ceramic substrate, then placing the glass or ceramic substrate in an oven for primary drying treatment, keeping the temperature at 105-120 ℃ for treatment for 30-45min, then placing the substrate in an atmospheric pressure plasma for treatment for 15-25min, then placing the substrate in the oven for final drying treatment, keeping the temperature at 185-195 ℃ for treatment for 45-60min, taking out and naturally cooling to room temperature, and the film material on the surface of the substrate is the novel sensor material.
On the basis of the technical scheme, the invention can be further improved as follows.
Specifically, the MXene material is Ti 3 C 2 Powder of Ti 2 C powder, ti 3 CN powder, V 4 C 3 Powder or V 2 One or more of C powder.
Specifically, the dosage ratio of aniline to ethanol in the aniline ethanol solution is 1-10g.
Specifically, the coating method of the liquid in the bottle on the substrate is spin coating or blade coating, and the thickness of the coating is 0.2-0.5mm.
Specifically, the atmospheric pressure plasma is generated by a dielectric barrier discharge device, the voltage is 11.2kV, the resistance is 75 omega, and the frequency is 690Hz.
The invention also provides a novel sensor material which is prepared by the method.
Compared with the prior art, the invention has the beneficial effects that:
the method comprises the steps of intercalating and surface modifying a two-dimensional MXene material by using ionic liquid and oxidized polyaniline formed by in-situ polymerization, and conducting diffusion under the voltage guide of a dielectric barrier discharge device and the polymerization and diffusion promotion effect of atmospheric pressure plasma in the intercalation modification and in-situ polymerization processes, so that the sensing performance of the two-dimensional MXene material on NOx gas is remarkably improved after the intercalation modification, and the response value at room temperature is more than 80.
Detailed Description
The principles and features of this invention are described below in conjunction with specific embodiments, which are provided for the purpose of illustration only and are not intended to limit the scope of the invention.
For the sake of avoiding redundant description, the raw materials used in the following examples are all commercially available products unless otherwise specified, and the methods used are all conventional methods in the art unless otherwise specified.
The thickness of the ceramic or glass substrate used in the following examples was 1mm, and Ti used therefor 3 C 2 Powder and Ti 2 The C powder is a product sold by the Fushan Xin alkene science and technology.
Example 1
A preparation method of a novel sensor material comprises the following steps: dissolving 10mL of 1-butyl-3-methylimidazolium iron tetrachloride ionic liquid in 50mL of pure water at room temperature to form an ionic liquid aqueous solution, and adding 1g of Ti in mass to the ionic liquid aqueous solution 3 C 2 Fully dispersing powder (MXene material) to obtain a mixed solution, dropwise adding an ethanol solution of aniline (2 g of aniline is dissolved in 50mL of ethanol) into the mixed solution at room temperature, stirring, wherein the stirring speed is 120r/min, the aniline is dropwise added within about 55min, stirring and reacting at a constant speed for 3h, performing reduced pressure rotary evaporation and concentration until the liquid in the bottle is reduced by about one third of the original volume (the liquid viscosity is obviously increased and the wall is obviously hung), coating the liquid in the bottle on a ceramic substrate, wherein the wet film thickness is about 0.3mm, then placing the ceramic substrate in an oven for primary drying treatment, keeping the temperature at 105-110 ℃ for 45min, placing the substrate between two polar plates of a dielectric barrier discharge device (the working voltage is 11.2kV, the resistance is 75 omega, the frequency is 690 Hz), placing the ceramic substrate in an atmospheric pressure plasma for treatment for 20min, placing the ceramic substrate in the oven for final drying treatment, keeping the temperature at 190-195 ℃ for 45min, taking out and naturally cooling to room temperature, wherein the film material on the surface of the substrate is the novel sensor material.
Example 2
A preparation method of a novel sensor material comprises the following steps: dissolving 10mL of 1-butyl-3-methylimidazolium iron tetrachloride ionic liquid in 60mL of pure water at room temperature to form an ionic liquid aqueous solution, and adding 0.5g Ti by mass to the ionic liquid aqueous solution 3 C 2 Fully dispersing the powder (MXene material) to obtain a mixed solution, and adding the mixed solution into the mixed solution at room temperatureDropwise adding an ethanol solution of aniline (2.5 g of aniline dissolved in 50mL of ethanol), stirring at the stirring speed of 135r/min for about 62min, maintaining the above rotation speed after dropwise adding for stirring reaction for 2h, then performing reduced pressure rotary evaporation and concentration until the liquid in the bottle is reduced to about one third of the original volume (the liquid viscosity is obviously increased and the wall hanging is obvious), coating the liquid in the bottle on a ceramic substrate, the wet film thickness is about 0.3mm, then placing the bottle in an oven for primary drying treatment, keeping the temperature at 115-120 ℃ for treatment for 30min, then placing the substrate between two polar plates of a dielectric barrier discharge device (the working voltage is 11.2kV, the resistance is 75 omega and the frequency is 690 Hz), treating the bottle under atmospheric pressure plasma for 25min, then placing the bottle in an oven for final drying treatment, keeping the temperature at 185-190 ℃ for treatment for 50min, taking out and naturally cooling the bottle to room temperature, thus obtaining the novel sensor material.
Example 3
A preparation method of a novel sensor material comprises the following steps: dissolving 10mL of 1-butyl-3-methylimidazolium iron tetrachloride ionic liquid in 80mL of pure water at room temperature to form an ionic liquid aqueous solution, and adding 1.5g of Ti by mass to the ionic liquid aqueous solution 3 C 2 Fully dispersing powder (MXene material) to obtain a mixed solution, dropwise adding an ethanol solution of aniline (7 g of aniline is dissolved in 50mL of ethanol) into the mixed solution at room temperature, stirring at a rotation speed of 150r/min for about 110min, maintaining the rotation speed after dropwise adding for stirring reaction for 3h, then carrying out reduced pressure rotary evaporation and concentration until the volume of liquid in a bottle is reduced to about one fourth of the original volume (the viscosity of the liquid is obviously increased and the wall is obviously hung), coating the liquid in the bottle on a ceramic substrate, wherein the thickness of a wet film is about 0.3mm, then placing the ceramic substrate in an oven for primary drying treatment, keeping the temperature at 105-120 ℃ for 40min, then placing the substrate between two polar plates of a dielectric barrier discharge device (the working voltage is 11.2kV, the resistance is 75 omega and the frequency is 690 Hz), carrying out atmospheric pressure plasma treatment for 25min, then placing the ceramic substrate in the oven for final drying treatment, keeping the temperature at 190-195 ℃ for 60min, taking out natural cooling to room temperature, and obtaining the film material on the surface of the substrate, namely the novel sensor material.
Example 4
Preparation method of novel sensor materialA method comprising the steps of: dissolving 10mL of 1-butyl-3-methylimidazolium iron tetrachloride ionic liquid in 55mL of pure water at room temperature to form an ionic liquid aqueous solution, and adding Ti with the mass of 0.75g to the ionic liquid aqueous solution 2 Fully dispersing C powder (MXene material) to obtain a mixed solution, dropwise adding an ethanol solution of aniline (1.5 g of aniline is dissolved in 50mL of ethanol) into the mixed solution at room temperature, stirring, wherein the stirring speed is 120r/min, the dropwise adding is completed within about 58min, stirring and reacting at the above rotating speed for 2h after the dropwise adding is completed, then carrying out reduced pressure rotary evaporation and concentration until the liquid in the bottle is reduced by about one third of the original volume (the liquid viscosity is obviously increased and the wall hanging is obvious), coating the liquid in the bottle on a glass substrate, wherein the wet film thickness is about 0.4mm, then placing the glass substrate in an oven for primary drying treatment, keeping the temperature at 105-110 ℃ for 45min, then placing the substrate between two polar plates of a dielectric barrier discharge device (the working voltage is 11.2kV, the resistance is 75 omega, and the frequency is 690 Hz), carrying out treatment under atmospheric pressure plasma for 18min, placing the glass substrate in the oven for final drying treatment, keeping the temperature at 190-195 ℃ for 50min, taking out, and naturally cooling to room temperature, wherein the film on the surface of the substrate is the novel sensor material.
Example 5
A preparation method of a novel sensor material comprises the following steps: dissolving 10mL of 1-butyl-3-methylimidazolium iron tetrachloride ionic liquid in 70mL of pure water at room temperature to form an ionic liquid aqueous solution, and adding 1.2g of Ti by mass to the ionic liquid aqueous solution 2 Fully dispersing C powder (MXene material) to obtain a mixed solution, dropwise adding an ethanol solution of aniline (5 g of aniline is dissolved in 50mL of ethanol) into the mixed solution at room temperature, stirring at a rotation speed of 130r/min within about 110min, maintaining the rotation speed after dropwise adding for stirring reaction for 3h, concentrating by reduced pressure rotary evaporation until the volume of the liquid in the bottle is reduced to about one third of the original volume (the viscosity of the liquid is obviously increased and the wall is obviously hung), coating the liquid in the bottle on a glass substrate, wherein the thickness of a wet film is about 0.5mm, primarily drying in an oven, keeping the temperature of 110-115 ℃ for 35min, and then placing the substrate between two polar plates (the working voltage is 11.2kV, the resistance is 75 omega and the frequency is 690 Hz) of a dielectric barrier discharge device under atmospheric pressure plasmaTreating for 20min, placing in an oven for final drying treatment, keeping at 185-190 ℃ for 60min, taking out, naturally cooling to room temperature, and obtaining the novel sensor material as the film material on the surface of the substrate.
Comparative example 1
As in example 1, except that after the preliminary baking treatment was completed, the atmospheric plasma treatment was not performed, but the substrate was directly transferred to an oven at 190 to 195 ℃ to be subjected to a final baking treatment for 45 minutes.
Comparative example 2
The same as example 2, except that the atmospheric plasma treatment was not performed after the preliminary baking treatment was completed, but the final baking treatment was performed.
Comparative example 3
The same as in example 3, except that the atmospheric plasma treatment was not performed after the preliminary baking treatment was completed, the final baking treatment was performed.
Performance testing
Preparing a gas sensor, preparing the novel sensor material by using the method of each embodiment and preparing the corresponding gas sensor at the same time, namely replacing the substrate in each embodiment with a 10 multiplied by 15mm ceramic wafer with a gold finger electrode, and finally drying to obtain the gas sensor using the corresponding novel sensor material. The gas-sensitive performance of the sensor corresponding to each embodiment was tested by using a gas-sensitive testing device assembled with a B2901A precision type power supply/measurement unit, the testing was performed at room temperature and atmospheric pressure, and the sensors were placed in 10ppmNO respectively during the testing 2 、50ppmHCHO、50ppmCO、50ppmSO 2 And 50ppmNH 3 The test results of the room temperature response value obtained by the test in the environment of (1) are shown in the following table:
as can be seen from the above table, the novel sensor material provided by the present invention is for NO 2 Gases have a significantly higher sensitivity than other interfering gases: the response value at room temperature can reach more than 80 when the concentration is 10ppm, and the rest gas is in the same conditionThe response values at room temperature of 50ppm are all below 3. Measured for NO in comparative examples 1 to 3 2 Compared with the corresponding examples, the response value of the gas shows that the atmospheric pressure plasma treatment has key effects on intercalation diffusion of the ionic liquid into the MXene material, final polymerization of aniline and intercalation diffusion into the MXene material, and the NO is obviously enhanced 2 Sensitivity to gases.
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, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (6)
1. A preparation method of a novel sensor material is characterized by comprising the following steps: mixing imidazole ionic liquid 1-butyl-3-methylimidazole ferric chloride salt and pure water at room temperature according to the weight ratio of 1:5-8, mixing and dissolving to form an ionic liquid aqueous solution, adding MXene material into the ionic liquid aqueous solution, and fully dispersing to obtain a mixed solution, wherein the dosage ratio of the MXene material to the 1-butyl-3-methylimidazole iron tetrachloride salt is 0.05-0.15g:1mL, adding an ethanol solution of aniline dropwise into the mixed solution at room temperature, and stirring, wherein the mass ratio of aniline to MXene in the mixed solution is (2-5): 1, stirring and reacting for 1-3h after finishing dripping, then decompressing, rotating, evaporating and concentrating until the liquid in the bottle is reduced to be less than one third of the original volume, coating the liquid in the bottle on a glass or ceramic substrate, then placing the glass or ceramic substrate in an oven for primary drying treatment, keeping the temperature at 105-120 ℃ for treatment for 30-45min, then placing the substrate in an atmospheric pressure plasma for treatment for 15-25min, then placing the substrate in the oven for final drying treatment, keeping the temperature at 185-195 ℃ for treatment for 45-60min, taking out and naturally cooling to room temperature, and the film material on the surface of the substrate is the novel sensor material.
2. The method for preparing the novel sensor material as claimed in claim 1, wherein the MXene material is Ti 3 C 2 Powder of Ti 2 C powder, ti 3 CN powder, V 4 C 3 Powder or V 2 One or more of C powder.
3. The method of claim 1, wherein the ratio of aniline to ethanol in the ethanol solution of aniline is 1-10g.
4. The preparation method of the novel sensor material according to claim 1, wherein the liquid in the bottle is coated on the substrate by spin coating or blade coating, and the thickness of the coating is 0.2-0.5mm.
5. The method of any one of claims 1 to 4, wherein atmospheric pressure plasma is generated by a dielectric barrier discharge device with a voltage of 11.2kV, a resistance of 75 Ω and a frequency of 690Hz.
6. A novel sensor material, characterized by being prepared by the method of any one of claims 1 to 5.
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