CN112763551A - Nitrogen dioxide sensor based on composite material blocking effect and preparation method thereof - Google Patents
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Abstract
The invention provides a nitrogen dioxide sensor based on composite material blocking effect and a preparation method thereof, which relate to the technical field of gas sensors and composite nano materials and comprise a sensitive device, wherein the sensitive device is provided with a gas-sensitive layer, and the gas-sensitive layer is made of a composite material with the blocking effect; the preparation method comprises the following steps: s1, preprocessing the sensitive device substrate, including cleaning, drying and hydrophilic processing; s2, preparing a high molecular polymer dispersion liquid and an inorganic conductive material dispersion liquid; s3, depositing the sensitive material dispersion liquid on the sensor substrate to form a gas-sensitive layer; and S4, drying and aging the sensitive device with the gas sensitive layer to obtain the nitrogen dioxide sensor based on the composite material blocking effect. The nitrogen dioxide sensor has the characteristics of large response, high response/recovery speed, good recovery, good repeatability and the like, can work at room temperature, does not need auxiliary means such as illumination or heating and the like, and is beneficial to the development of green energy-saving and low-power-consumption devices.
Description
Technical Field
The invention relates to the technical field of gas sensors and composite nano materials, in particular to a nitrogen dioxide sensor based on a composite material blocking effect and a preparation method thereof.
Background
Nitrogen dioxide (NO), a toxic and irritating gas2) Is a main atmospheric pollutant, can cause the reduction of atmospheric visibility, the acidification of surface water, eutrophication and the increase of the toxin content of aquatic organisms; in addition, NO2After being inhaled by human body, the medicine has strong irritation and corrosiveness to lung tissue. Thus, development of NO2Gas sensors are of great significance.
At present, NO2Most of gas sensors are based on an electron transport mechanism, for example, the invention patent with the application number of 201910276010.0 discloses a nitrogen dioxide sensor based on a two-dimensional molybdenum disulfide nano material, under the irradiation of ultraviolet light, molybdenum disulfide arranged between a source electrode and a drain electrode adsorbs NO2After gassing, NO2The gas molecules capture electrons from the molybdenum disulfide, causing a change in the conductance of the sensor. Molybdenum disulfide based gas sensors, while having a lower detection limit, have recovery times of less than 200s and require light assist. The invention patent of application No. 202010017845.7 discloses a gold-modified flower-shaped SnS2 nitrogen dioxide gas sensor and a preparation method thereof. The nitrogen dioxide gas sensor comprises a gas sensitive material and a heating electrode, wherein flower-shaped SnS2 with gold uniformly distributed is coated on the surface of the heating electrode. The sensor is paired with 8ppm NO2The response value was about 15, the response time was 120.8s, and the recovery time was 249.4 s. Although many NO based on electron transport mechanisms2The gas sensor has better gas-sensitive performance, but the gas sensor with high response, high speed, good repeatability and good reversibility is developed at room temperatureBut is a challenge.
Disclosure of Invention
The invention provides a nitrogen dioxide sensor based on a composite material blocking effect and a preparation method thereof, which are used for solving the problems of poor performance and high power consumption of a gas sensor at room temperature in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the nitrogen dioxide sensor based on the blocking effect of the composite material comprises a sensitive device, wherein a gas sensitive layer is arranged on the sensitive device and is made of the composite material with the blocking effect;
the blocking effect is that gas molecules are adsorbed on the surface of a sensitive material through non-covalent bonds to block ion conduction, so that the resistance of the sensor is increased;
the composite material is a high molecular polymer inorganic conductive material, the high molecular polymer is represented by gamma-polyglutamic acid, the high molecular polymer has functional groups such as amino, carboxyl, amido bond or hydroxyl, and the high molecular polymer is dynamically adsorbed/desorbed by forming non-covalent bonds with gas molecules; the inorganic conductive material is represented by an MXene material, and the inorganic conductive material includes a carbon-based material having a three-dimensional support structure;
the structural formula of the MXene material is Mn+1XnOr Mn+1XnTx(n-1-3) wherein M represents a transition metal, X represents carbon and/or nitrogen, TxRepresents a terminal functional group.
Further, the carbon-based material includes single-walled or multi-walled carbon nanotubes, carbon fibers, graphene and derivatives thereof, and carbon black.
Further, the sensitive device is an interdigital electrode of a rigid or flexible substrate.
Further, when the sensitive device is an interdigital electrode with a rigid base, a rigid silicon-based substrate or a ceramic substrate or an aluminum oxide substrate is adopted, and when the sensitive device is an interdigital electrode with a flexible base, one of flexible Polyimide (PI), polyethylene terephthalate (PET), Polyurethane (PU), a cloth base and a paper base is adopted.
Furthermore, the number of the interdigital electrodes is 1-50 pairs, and the fork value spacing of each pair of the interdigital electrodes is 5-500 μm.
Further, the gas-sensitive layer has a thickness of 50nm to 500 μm.
The preparation method of the nitrogen dioxide sensor based on the blocking effect of the composite material comprises the following steps:
s1, preprocessing the sensitive device substrate, including washing, drying and hydrophilic processing;
s2, preparing a high molecular polymer dispersion liquid and an inorganic conductive material dispersion liquid;
s3, depositing the sensitive material dispersion liquid on the sensor substrate to form a gas-sensitive layer;
and S4, drying and aging the sensitive device with the gas sensitive layer to obtain the nitrogen dioxide sensor based on the composite material blocking effect.
Furthermore, the solvent of the sensitive material dispersion liquid is one of deionized water, ethanol, acetone and N-methyl pyrrolidone.
Further, the deposition process of the gas-sensitive layer includes a process of coating with a paint pen, spray coating, spin coating, drop coating, dip coating, or self-assembly.
Further, the gas-sensitive layer is a single-layer or multi-layer film.
Compared with the prior art, the invention has the beneficial effects that:
(1) in the invention, the gas-sensitive property of the inorganic conductive material represented by MXene is improved by combining the blocking effect of the high molecular polymer, so that the nitrogen dioxide sensor has the characteristics of large response, high response/recovery speed, good recovery, good repeatability and the like.
(2) In the invention, the nitrogen dioxide sensor based on the composite material blocking effect can work at room temperature without auxiliary means such as illumination or heating, and is beneficial to the development of green energy-saving and low-power-consumption devices.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments of the present invention will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 shows a view of modification of titanium carbide (Ti) with gamma-polyglutamic acid in the present invention2C3Tx) Scanning electron microscope images of the composite film;
FIG. 2 shows the modification of Ti with gamma-polyglutamic acid in the present invention2C3TxA real-time change curve diagram of the resistance of the composite film sensor;
FIG. 3 shows the modification of Ti with gamma-polyglutamic acid in the present invention2C3TxA composite film sensor response time plot;
FIG. 4 shows the modification of Ti with gamma-polyglutamic acid in the present invention2C3TxA repeatability curve graph of the composite film sensor;
FIG. 5 is a graph showing the real-time variation of the resistance of the gamma-polyglutamic acid modified multi-walled carbon nanotube (MWCNTs) composite thin film sensor of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention.
Example 1
The sensing device selected in the embodiment is a flexible interdigital electrode, the interdigital electrode is a gold electrode manufactured on a flexible Polyimide (PI) substrate, the interdigital distance of the interdigital electrode is 200 microns, the interdigital width of the interdigital electrode is 200 microns, and the electrode thickness of the interdigital electrode is 100 nm; in the embodiment, a gamma-polyglutamic acid/Ti 2C3Tx composite material is used as a gas sensitive material, and a drop coating process is adopted to prepare a composite film sensitive layer, wherein the specific process steps are as follows:
(1) pretreating a PI substrate gold interdigital electrode, and cleaning with ionized water, acetone, alcohol and deionized water; drying for later use;
(2) preparing gamma-polyglutamic acid dispersion liquid, wherein a solvent is deionized water, preparing the gamma-polyglutamic acid dispersion liquid with the concentration of 1mg/mL, and performing ultrasonic treatment for later use;
(3) preparation of less-layer Ti2C3TxNanosheets. To etch phase precursors (Ti)3AlC2) Adopts a two-step method to synthesize Ti as raw material2C3TxNanosheets. 15mL of deionized water and 10mL of 40% aqueous HF were added to the beaker, and 1g of Ti was slowly added over 1min3AlC2And (3) performing ultrasonic treatment on the powder for 15min to fully mix the powder with the etching solution. Stirring for 2h at room temperature, centrifuging and cleaning until the pH value reaches 6-7 to obtain Ti2C3TxAnd (5) primary product. Then, 15mL of 25 wt.% aqueous tetramethylammonium hydroxide (TMAOH) solution was added to the above precipitate for further etching and intercalation. Stirring for 4h at 35 ℃, and centrifugally collecting Ti2C3TxThe slurry was washed cyclically with deionized water (6000rpm) to remove excess TMAOH. Finally removing excessive water molecules by using a freeze drying method, and collecting few layers of Ti after grinding2C3TxAnd (3) powder.
(4) Preparation of Gamma-polyglutamic acid/Ti2C3TxMeasuring 10mg of the prepared few-layer Ti2C3TxAdding the powder into 15mL of gamma-PGA aqueous solution, and carrying out ultrasonic treatment at room temperature for 10min for later use.
(5) Preparing a gas-sensitive composite film on an interdigital electrode of a flexible PI substrate by a drop coating process; drying at 60 ℃ for 12h to obtain the gamma-polyglutamic acid/Ti2C3Tx NO2A gas sensor.
Example 2
The sensing device selected in the embodiment is a flexible interdigital electrode, the interdigital electrode is a gold electrode manufactured on a flexible Polyimide (PI) substrate, the interdigital distance of the interdigital electrode is 200 microns, the interdigital width of the interdigital electrode is 200 microns, and the electrode thickness of the interdigital electrode is 100 nm; in the embodiment, a gamma-polyglutamic acid/multi-walled carbon nanotube (MWCNTs) composite material is selected as a gas sensitive material, and a spraying process is adopted to prepare a composite film sensitive layer, wherein the specific process steps are as follows:
(1) pretreating a PI substrate gold interdigital electrode, and cleaning with ionized water, acetone, alcohol and deionized water; drying for later use;
(2) preparing gamma-polyglutamic acid dispersion liquid, wherein a solvent is deionized water, preparing the gamma-polyglutamic acid dispersion liquid with the concentration of 1mg/mL, and performing ultrasonic treatment for later use;
(3) MWCNTs dispersion liquid is prepared. The solvent is deionized water, MWCNTs dispersion liquid with the concentration of 0.5 wt% is prepared, and the MWCNTs dispersion liquid is subjected to ultrasonic treatment for later use.
(4) Preparing the gamma-polyglutamic acid/MWCNTs composite solution, measuring 1mL MWCNTs dispersion liquid, adding into 10mL gamma-polyglutamic acid dispersion liquid, and carrying out ultrasonic treatment at room temperature for 10min for later use.
(5) Spraying 0.2mL of mixed solution on an interdigital electrode of a flexible PI substrate to prepare a gas-sensitive composite membrane; drying for 12h at the temperature of 60 ℃ to obtain the gamma-polyglutamic acid/MWCNTs NO2A gas sensor.
Example 3
In the embodiment, a sensitive device is selected as a flexible interdigital electrode, the interdigital electrode is a nickel-chromium-gold electrode on a flexible PET substrate, the interdigital distance of the interdigital electrode is 50 μm, the interdigital width is 50 μm, and the electrode thickness is 100 nm; in the embodiment, a gamma-polyglutamic acid/carbon nanofiber composite material is selected as a gas sensitive material, and a drop coating process is adopted to prepare a composite film sensitive layer, wherein the specific process steps are as follows:
(1) pretreating the nickel-chromium-gold interdigital electrode of the PET substrate, and cleaning with ionized water, acetone, alcohol and deionized water; drying, and performing ultraviolet hydrophilic treatment for 10 min;
(2) preparing gamma-polyglutamic acid dispersion liquid, wherein a solvent is deionized water, preparing the gamma-polyglutamic acid dispersion liquid with the concentration of 1mg/mL, and performing ultrasonic treatment for later use;
(3) preparing gamma-polyglutamic acid/carbon nanofiber composite solution, measuring 10mg of carbon nanofiber powder, adding into 10mL of gamma-polyglutamic acid dispersion liquid, and carrying out ultrasonic treatment at room temperature for 10min for later use.
(4) Preparing a gas-sensitive composite film on an interdigital electrode of a flexible PET substrate by a drop coating process; drying for 12h at the temperature of 60 ℃ to obtain the gamma-polyglutamic acid/carbon nanofiber NO2A gas sensor.
Test example 1
Gamma-polyglutamic acid/Ti prepared according to example 12C3TxComposite film NO2The sensor, performance test was performed according to methods known in the art. The specific method comprises the following steps: the resistance signals of the above prepared sensors were tested in a simulated atmospheric environment (50% RH) using an AES-4SD device analyzer, with different NO2The concentration is obtained by gas dilution method, and the tested concentration is 2-50 ppm.
The technical scheme of the invention is that the prepared gamma-polyglutamic acid modifies Ti2C3TxThe scanning electron microscope image of the composite film is shown in FIG. 1, and the composite film has a nanosheet structure Ti2C3TxThe two-dimensional material can promote the gas adsorption sites of the composite film. The gamma-polyglutamic acid adsorbs gas molecules through non-covalent bonds, and the composite material can improve the effective adsorption of the sensor.
FIG. 2 shows gamma-polyglutamic acid modified Ti2C3TxThe resistance of the composite film sensor changes in real time under 2-50 ppm. As shown in the figure, NO2Upon passing, the sensor exhibited a positive resistance response behavior. As the gas concentration increases, the resistance of the sensor increases. And gamma-polyglutamic acid modified Ti2C3TxThe composite film sensor shows large response value (to 50ppm NO)2Response up to 1136%), the resistance quickly approaches steady state.
FIG. 3 shows gamma-polyglutamic acid modified Ti2C3TxComposite thin film sensor response time plot. As shown, the sensor is paired with 50ppm NO2Exhibit excellent response/recovery speed; the response time was calculated to be about 25s and the recovery time was calculated to be about 3 s.
FIG. 4 shows the modification of Ti by gamma-polyglutamic acid2C3TxA composite film sensor repeatability curve. As shown, the sensor has good repeatability, and the Relative Standard Deviation (RSD) of the sensor is about 0.94% by calculating six steady state response values.
Test example 2
Gamma-polyglutamic acid/MWCNT prepared according to example 2s composite film NO2The sensor, performance test was performed according to methods known in the art. The specific method comprises the following steps: the resistance signals of the above prepared sensors were tested in a simulated atmospheric environment (50% RH) using an AES-4SD device analyzer, with different NO2The concentration was obtained by gas dilution and was tested at 10-50 ppm.
The technical scheme of the invention is that the prepared gamma-polyglutamic acid modified MWCNTs composite film NO2Sensor pair 10-50ppm NO2The real-time resistance change curve is shown in fig. 5. NO2Upon passing, the sensor exhibited a positive resistance response behavior. As the gas concentration increases, the resistance of the sensor increases. The sensor also showed high response (to 50ppm NO)2Response 541%) and short response/recovery time (-28 s/3 s).
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The nitrogen dioxide sensor based on the blocking effect of the composite material is characterized by comprising a sensitive device, wherein a gas-sensitive layer is arranged on the sensitive device and is made of the composite material with the blocking effect;
the blocking effect is that gas molecules are adsorbed on the surface of a sensitive material through non-covalent bonds to block ion conduction, so that the resistance of the sensor is increased;
the composite material is a high molecular polymer inorganic conductive material, the high molecular polymer is represented by gamma-polyglutamic acid, the high molecular polymer has amino, carboxyl, amido bond or hydroxyl functional group, and the high molecular polymer is dynamically adsorbed/desorbed by forming a non-covalent bond with gas molecules; the inorganic conductive material is represented by an MXene material, and the inorganic conductive material includes a carbon-based material having a three-dimensional support structure;
the MXene material has a structural formula ofMn+1XnOr Mn+1XnTx(n-1-3) wherein M represents a transition metal, X represents carbon and/or nitrogen, TxRepresents a terminal functional group.
2. The composite occlusion effect based nitrogen dioxide sensor of claim 1, wherein the carbon-based material comprises single or multi-walled carbon nanotubes, carbon fibers, graphene and its derivatives, carbon black.
3. The nitrogen dioxide sensor based on composite blocking effect according to claim 1, wherein the sensitive device is an interdigital electrode of a rigid or flexible substrate.
4. The nitrogen dioxide sensor based on composite blocking effect according to claim 3, wherein when the sensitive device is an interdigital electrode with a rigid base, a rigid silicon-based substrate or a ceramic substrate or an aluminum oxide substrate is adopted, and when the sensitive device is an interdigital electrode with a flexible base, one of flexible Polyimide (PI), polyethylene terephthalate (PET), Polyurethane (PU), a cloth base and a paper base is adopted.
5. The nitrogen dioxide sensor based on composite blocking effect according to claim 3, wherein the number of the interdigital electrodes is 1-50 pairs, and the fork value spacing of each pair of fork value electrodes is 5-500 μm.
6. The nitrogen dioxide sensor based on composite blocking effect according to claim 1, wherein the gas-sensitive layer has a thickness of 50nm-500 μm.
7. A method for preparing a nitrogen dioxide sensor based on the blocking effect of a composite material according to any one of claims 1 to 6, which comprises the following steps:
s1, preprocessing the sensitive device substrate, including washing, drying and hydrophilic processing;
s2, preparing a high molecular polymer dispersion liquid and an inorganic conductive material dispersion liquid;
s3, depositing the sensitive material dispersion liquid on the sensor substrate to form a gas-sensitive layer;
and S4, drying and aging the sensitive device with the gas sensitive layer to obtain the nitrogen dioxide sensor based on the composite material blocking effect.
8. The method for preparing a nitrogen dioxide sensor based on composite material blocking effect according to claim 7, wherein the solvent of the sensitive material dispersion in step S3 is one of deionized water, ethanol, acetone and N-methylpyrrolidone.
9. The method for preparing a nitrogen dioxide sensor based on composite material blocking effect according to claim 7, wherein the deposition process of the gas-sensitive layer in step S3 includes a process of coating with a paint pen, spraying, spin coating, drop coating, dip coating or self-assembly.
10. The method for preparing a nitrogen dioxide sensor based on composite material blocking effect according to claim 7, wherein the gas sensitive layer in step S3 is a single-layer or multi-layer film.
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| CN115259156A (en) * | 2022-07-18 | 2022-11-01 | 微集电科技(苏州)有限公司 | Capable of detecting low concentration NO at room temperature2Gas sensitive element and preparation method thereof |
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| CN115259156A (en) * | 2022-07-18 | 2022-11-01 | 微集电科技(苏州)有限公司 | Capable of detecting low concentration NO at room temperature2Gas sensitive element and preparation method thereof |
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