CN113552182A - Preparation method of flexible gas sensor for fabric - Google Patents
Preparation method of flexible gas sensor for fabric Download PDFInfo
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- CN113552182A CN113552182A CN202110837099.0A CN202110837099A CN113552182A CN 113552182 A CN113552182 A CN 113552182A CN 202110837099 A CN202110837099 A CN 202110837099A CN 113552182 A CN113552182 A CN 113552182A
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- fabric
- coating solution
- gas sensor
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- sensor
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- G—PHYSICS
- 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
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/126—Composition of the body, e.g. the composition of its sensitive layer comprising organic polymers
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/007—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by mechanical or physical treatments
- D06N3/0077—Embossing; Pressing of the surface; Tumbling and crumbling; Cracking; Cooling; Heating, e.g. mirror finish
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/04—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
Abstract
The invention relates to a preparation method of a flexible gas sensor for fabric, which comprises the following steps of selecting an area on the fabric as a sensor processing area; step two, preparing a coating solution by using the mass ratio of the alcohol-soluble phenolic resin to the poloxamer of more than 1:2 and less than or equal to 2:1, wherein the mass ratio of the sum of the mass of the alcohol-soluble phenolic resin and the poloxamer to the absolute ethyl alcohol is 1: 4; placing the coating solution in a vacuum box for degassing treatment, spin-coating the degassed coating solution on a sensor processing area of the fabric, and placing the fabric spin-coated with the coating solution in a vacuum drying box for vacuum heating and drying; fourthly, ablating the area of the dried fabric, which is coated with the coating solution in a spin mode, by using a carbon dioxide laser to obtain porous carbon; and respectively sticking electrode plates at two ends of the region where the porous carbon is located. The gas sensor is combined with the fabric, so that the flexibility and the air permeability of the fabric are maintained, and the manufacturing cost of the intelligent protective clothing is reduced.
Description
Technical Field
The invention belongs to the technical field of sensor preparation, and particularly relates to a preparation method of a flexible gas sensor for fabrics.
Background
Most of the traditional gas sensors use rigid materials as substrates and metal oxides as gas sensitive materials. With the rapid development of the manufacturing technology of the flexible device, the gas sensitive material can be coated on a flexible substrate such as a polyimide film (PI), a polyethylene terephthalate film (PET), and polyimide by spin coating, printing, and the like, so as to prepare the flexible gas sensor. Compared with a rigid sensor, the flexible gas sensor is easier to integrate into systems such as a multi-sensor array, an electronic nose, an intelligent textile, an industrial radio frequency tag and the like so as to meet the development trend of miniaturization, intelligence and multiple functions of the gas sensor.
In some high-risk industrial environments, toxic and harmful gases generated by leakage show a colorless and tasteless state at low concentration, but can also cause irreversible damage to a human body, so that workers are required to wear intelligent protective clothing, and the toxic and harmful gases are detected in real time through a gas sensor, so that the safety protection is facilitated, and the leakage can be found in time.
At present mainly wear gas sensor on intelligent protective clothing through wearable equipment, not only dress is inconvenient, influences the gas permeability and the travelling comfort of protective clothing moreover, consequently how to integrate gas sensor to the protective clothing when keeping original flexibility of fabric and gas permeability, is the technical problem that intelligent protective clothing needs to solve.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a flexible gas sensor for fabric.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method of making a flexible gas sensor for use with a textile fabric, the method comprising the steps of:
step one, selecting an area on a fabric as a sensor processing area;
step two, preparing a coating solution by taking alcohol-soluble phenolic resin, poloxamer and absolute ethyl alcohol as raw materials; wherein the mass ratio of the alcohol-soluble phenolic resin to the poloxamer is more than 1:2 and less than or equal to 2:1, and the mass ratio of the sum of the mass of the alcohol-soluble phenolic resin and the poloxamer to the absolute ethyl alcohol is 1: 4;
placing the coating solution in a vacuum box for degassing treatment, spin-coating the degassed coating solution on a sensor processing area of the fabric, and then placing the fabric spin-coated with the coating solution in a vacuum drying box for vacuum heating and drying;
fourthly, ablating the area of the dried fabric, which is coated with the coating solution in a spin mode, by using a carbon dioxide laser to obtain porous carbon; and respectively sticking electrode plates at two ends of the region where the porous carbon is located to finish the preparation of the gas sensor.
The poloxamer is block copolymer F127.
In the third step, the temperature for vacuum heating and drying is 100 ℃, and the time is 12-24 hours.
The spin coating process in the third step comprises the following steps: firstly, spreading a coating solution at a speed of 400 revolutions per minute by using a spin coater, wherein the time duration is 15 s; the coating solution was then spin coated uniformly at a rate of 800 revolutions per minute for 45 seconds.
The upper surface of the electrode plate is coated with a silver film.
The sensor comprises a flexible substrate, electrodes and a sensing area; the flexible substrate is a fabric, and the area where the porous carbon is located is a sensing area.
Compared with the prior art, the invention has the beneficial effects that:
1) the method comprises the steps of preparing a coating solution by taking a block copolymer (poloxamer) as a guide, coating the coating solution on a fabric in a spin coating mode, and ablating porous carbon by a carbon dioxide laser to obtain the gas sensor; the coating solution is combined with the common fabric, so that the original flexibility and air permeability of the fabric can be maintained, the sensor is tightly combined with the fabric and does not need to be combined with wearable equipment, the cost for manufacturing the intelligent protective clothing is reduced to a great extent, and an idea is provided for manufacturing textile electronic products.
2) The method can regulate and control the aperture size of the porous carbon by changing the mass ratio of the alcohol-soluble phenolic resin to the poloxamer, thereby changing the response rate of the gas sensor to the gas, and the method has the characteristics of regular and uniform pore arrangement and easy regulation and control. The invention is characterized in that the coating solution is directly combined with the fabric to obtain the flexible gas sensor, and the air permeability and the flexibility of the fabric are not influenced. The method has good repeatability, obvious detection effect and simple preparation process.
Drawings
FIG. 1 is a schematic representation of the attachment of a sensor of the present invention to a fabric;
FIG. 2 is an electron micrograph of the porous carbon obtained in example 1;
FIG. 3 is an electron micrograph of the porous carbon obtained in example 2;
FIG. 4 is an electron micrograph of a porous carbon obtained in a comparative example;
FIG. 5 is a continuous response graph of the sensor obtained in example 2 measuring NO gas;
FIG. 6 is a graph showing the repetitive response of the sensor obtained in example 2 measured in NO gas at a concentration of 2 ppm;
FIG. 7 is a graph showing a comparison of the response of the sensor obtained in example 2 in a non-bent and bent state in an NO gas concentration of 2 ppm;
fig. 8 is a graph showing the change in resistance of the sensor obtained in example 2 after bending for a plurality of cycles.
Detailed Description
The technical solution of the present invention is described in detail below with reference to the specific embodiments and the accompanying drawings, but the scope of the present invention is not limited thereto.
The invention relates to a preparation method (a method for short) of a flexible gas sensor for fabric, wherein the gas sensor comprises a flexible substrate, electrodes and a sensing area;
the method comprises the following steps:
selecting an area on a fabric as a sensor processing area, wherein the fabric is used as a flexible substrate of a sensor;
step two, preparing a coating solution by taking alcohol-soluble phenolic resin, poloxamer (polyoxyethylene polyoxypropylene ether block copolymer) and absolute ethyl alcohol as raw materials; wherein the mass ratio of the alcohol-soluble phenolic resin to the poloxamer is more than 1:2 and less than or equal to 2:1, and the mass ratio of the sum of the mass of the alcohol-soluble phenolic resin and the poloxamer to the absolute ethyl alcohol is 1: 4;
step three, placing the coating solution in a vacuum box for degassing treatment to remove bubbles in the solution; dripping the coating solution subjected to degassing treatment on a sensor processing area of the fabric by using an injector, and carrying out spin coating by using a spin coater; then putting the fabric coated with the coating solution in a vacuum drying oven for vacuum heating and drying; the drying time is 12-24 h;
fourthly, ablating the area of the dried fabric, which is coated with the coating solution in a spinning mode, by using a carbon dioxide laser to obtain porous carbon, wherein the area where the porous carbon is located is a sensing area of the sensor; electrode plates are respectively stuck at two ends of the sensing area and are connected with the digital source meter to finish the preparation of the gas sensor; the gas causes a change in resistance in the sensing area, and the gas concentration is detected by the change in resistance.
The upper surface of the electrode plate is coated with the silver film, so that the resistance can be obviously reduced, and the power consumption of the dead work of the sensor can be reduced; in addition, the silver thin film may also function as a protective electrode.
Poloxamer is preferably block copolymer F127.
Example 1
The preparation method of the flexible gas sensor for the fabric comprises the following steps:
selecting an area on a fabric as a sensor processing area, wherein the fabric is used as a flexible substrate of a sensor;
step two, according to the mass ratio of 2:1, respectively weighing alcohol-soluble phenolic resin and a block copolymer F127, wherein the alcohol-soluble phenolic resin and the block copolymer F127 are used as solutes, and the mass ratio of the solutes to the solvent is 1:4, weighing absolute ethyl alcohol according to the proportion, wherein the absolute ethyl alcohol is used as a solvent; pouring the weighed alcohol-soluble phenolic resin and block copolymer F127 into absolute ethyl alcohol for stirring, wherein the stirring temperature is 40 ℃, the stirring speed is 800 revolutions per minute, and the stirring time is 4 hours until the alcohol-soluble phenolic resin and the block copolymer F127 are completely fused, so as to prepare a coating solution;
step three, placing the coating solution in a vacuum box for degassing treatment for 0.5h, and removing bubbles in the coating solution; dripping the coating solution subjected to degassing treatment on a sensor processing area of the fabric by using an injector, and carrying out spin coating by using a spin coater; firstly, spreading the coating solution at a speed of 400 revolutions per minute by a spin coater for 15 s; uniformly spin-coating the solution at the speed of 800 revolutions per minute for 45 s; then putting the fabric coated with the coating solution in a vacuum drying oven for vacuum heating and drying, wherein the drying temperature is 100 ℃, and the drying time is 16 h;
fourthly, ablating the area of the dried fabric, which is coated with the coating solution in a spinning mode, by using a carbon dioxide laser to obtain porous carbon, wherein the area where the porous carbon is located is a sensing area; electrode plates are respectively stuck at two ends of the sensing area and are connected with the digital source meter to finish the preparation of the gas sensor; wherein, the power of the carbon dioxide laser is 3W, the speed is 13-15 mm/s, and the porous carbon generated under the power and the speed has the best response to gas.
FIG. 2 is an electron microscope image of the porous carbon obtained in this example, and a carbon dioxide laser is used to ablate the coated area of the fabric to form a regular porous structure with a pore size of 50-150 nm.
Example 2
In this embodiment, except that the ratio of the raw materials for preparing the coating solution in the second step is different from that in embodiment 1, the other steps are the same as in embodiment 1, and specifically, the following steps are performed:
according to the mass ratio of 1: 1, respectively weighing alcohol-soluble phenolic resin and a block copolymer F127, and then mixing the alcohol-soluble phenolic resin and the block copolymer F127 according to the mass ratio of a solute to a solvent of 1:4, anhydrous ethanol was weighed in proportion to prepare a coating solution.
FIG. 3 is an electron microscope image of the porous carbon obtained in this example, and a carbon dioxide laser is used to ablate the coated area of the fabric to form a regular porous structure with a pore size of 100-200 nm.
FIG. 5 is a continuous response chart of the sensor measuring NO gas obtained in the present embodiment, wherein R represents the resistance of the sensor after change in gas, and R is0Represents the initial resistance; as can be seen from the graph, as the gas concentration increases, the response amount of the sensor also increases, indicating that the sensitivity of the sensor is good.
Fig. 6 is a repeated response graph of the sensor obtained in the present example measured in NO gas with a concentration of 2ppm, and the gas concentration and the response amount of the sensor were not changed, so that the sensor had good reproducibility.
Fig. 7 is a graph showing a comparison of the response of the sensor obtained in the present example in a NO gas concentration of 2ppm in a non-bent state and in a bent state, in which the response of the sensor is good and the sensitivity of the sensor is not affected.
Fig. 8 is a graph showing the resistance change of the sensor obtained in the present example after multiple bending cycles, and it can be seen from the graph that the resistance of the sensor remains unchanged after the multiple bending cycles and the multiple unfolding cycles, indicating that the flexibility of the sensor is good.
Comparative example
In this embodiment, except that the ratio of the raw materials for preparing the coating solution in the second step is different from that in embodiment 1, the other steps are the same as in embodiment 1, and specifically, the following steps are performed:
according to the mass ratio of 1:2, respectively weighing the alcohol-soluble phenolic resin and the block copolymer F127, and then mixing the alcohol-soluble phenolic resin and the block copolymer F127 according to the mass ratio of the solute to the solvent of 1:4, anhydrous ethanol was weighed in proportion to prepare a coating solution.
FIG. 4 is an electron microscope image of the porous carbon obtained in the present example, and it can be seen from FIG. 4 that the pore diameter of the porous carbon is increased, but a regular porous structure is not formed, because the alcohol-soluble phenolic resin is polymerized and crosslinked to form a carbon skeleton during the laser ablation process, and the block copolymer F127 is decomposed to generate pores, which causes volume shrinkage; when the content of the alcohol-soluble phenol resin is too low, the volume shrinkage is large, the carbon skeleton is insufficient to support the porous structure, and collapse occurs, so that a regular porous structure cannot be formed.
In addition, as can be seen from examples 1 and 2 and the comparative example, the pore size of the porous carbon is increased with the increase of the content of poloxamer, so that the pore size of the porous carbon can be regulated and controlled by changing the mass ratio of the alcohol-soluble phenolic resin to the poloxamer, thereby changing the sensitivity of the gas sensor to the response of the gas.
Nothing in this specification is said to apply to the prior art.
Claims (6)
1. A method of making a flexible gas sensor for use with a textile fabric, the method comprising the steps of:
step one, selecting an area on a fabric as a sensor processing area;
step two, preparing a coating solution by taking alcohol-soluble phenolic resin, poloxamer and absolute ethyl alcohol as raw materials; wherein the mass ratio of the alcohol-soluble phenolic resin to the poloxamer is more than 1:2 and less than or equal to 2:1, and the mass ratio of the sum of the mass of the alcohol-soluble phenolic resin and the poloxamer to the absolute ethyl alcohol is 1: 4;
placing the coating solution in a vacuum box for degassing treatment, spin-coating the degassed coating solution on a sensor processing area of the fabric, and then placing the fabric spin-coated with the coating solution in a vacuum drying box for vacuum heating and drying;
fourthly, ablating the area of the dried fabric, which is coated with the coating solution in a spin mode, by using a carbon dioxide laser to obtain porous carbon; and respectively sticking electrode plates at two ends of the region where the porous carbon is located to finish the preparation of the gas sensor.
2. The method of claim 1, wherein the poloxamer is a block copolymer F127.
3. The preparation method of the flexible gas sensor for the fabric according to claim 1, wherein the temperature of vacuum heating and drying in the third step is 100 ℃, and the time is 12-24 hours.
4. The method for preparing a flexible gas sensor for fabric according to claim 1, wherein the spin coating in step three comprises: firstly, spreading a coating solution at a speed of 400 revolutions per minute by using a spin coater, wherein the time duration is 15 s; the coating solution was then spin coated uniformly at a rate of 800 revolutions per minute for 45 seconds.
5. The method for manufacturing a flexible gas sensor for fabric according to claim 1, wherein the upper surface of the electrode sheet is coated with a silver thin film.
6. The method for preparing a flexible gas sensor for fabric according to any one of claims 1 to 5, wherein the sensor comprises a flexible substrate, electrodes and a sensing area; the flexible substrate is a fabric, and the area where the porous carbon is located is a sensing area.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115420393A (en) * | 2022-09-06 | 2022-12-02 | 河北工业大学 | Preparation method of gas-temperature sensor |
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