CN111472165A - Polyaniline-coated carbon nanotube coating flexible electromagnetic shielding fabric and preparation method thereof - Google Patents
Polyaniline-coated carbon nanotube coating flexible electromagnetic shielding fabric and preparation method thereof Download PDFInfo
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- CN111472165A CN111472165A CN202010332324.0A CN202010332324A CN111472165A CN 111472165 A CN111472165 A CN 111472165A CN 202010332324 A CN202010332324 A CN 202010332324A CN 111472165 A CN111472165 A CN 111472165A
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Abstract
The invention discloses a polyaniline-coated carbon nanotube coating flexible electromagnetic shielding fabric and a preparation method thereof, belonging to the field of flexible electromagnetic shielding fabrics, wherein the method comprises the steps of coating a carbon nanotube subjected to carboxylation treatment on the surface of a pretreated fabric, polymerizing aniline on the surface of the fabric in situ, and coating the carbon nanotube with polyaniline to obtain the polyaniline-coated carbon nanotube coating flexible electromagnetic shielding fabric; the polyaniline is coated on the surface of the carboxylated carbon nano-coating fabric by an in-situ polymerization method, special equipment is not needed, the process is simple, the cost is low, the production efficiency is high, and the polyaniline can be produced in large scale in the existing textile printing and dyeing equipment; the method solves the double difficulties that polyaniline is difficult to dissolve in organic solvents and the carbon nano tube has poor dispersibility, effectively combines the advantages of polyaniline and the carbon nano tube, and plays a synergistic effect in the aspect of playing excellent electromagnetic shielding performance.
Description
Technical Field
The invention relates to the field of flexible electromagnetic shielding fabrics, in particular to a polyaniline-coated carbon nanotube coating flexible electromagnetic shielding fabric and a preparation method thereof.
Background
The electronic information technology is rapidly advanced, and the electromagnetic radiation pollution generated along with the electronic information technology is more and more serious. The preparation of the flexible high-efficiency electromagnetic shielding fabric is the key point of attention of material engineers. In the prior art, methods such as metal wire blending or interweaving, metal plating on the surface of fabric, polypyrrole or polyaniline coating, combination of the two and the like are adopted.
As described in patent CN109267199A, polyaniline-coated carbon nanotube fiber bundles are prepared first, and then polyaniline/carbon nanotube fiber composites are prepared by twisting. The composite material is a carbon nano tube fiber aggregate, and is obtained by compounding polyaniline and carbon nano tube fiber bundles.
As also disclosed in patent CN104005224N, a polyaniline-coated fabric is prepared, and then metal nickel is plated on the surface of the polyaniline-coated fabric to prepare the wave-absorbing electromagnetic shielding fabric.
In patent CN104846620B, polyaniline is grafted on the surface of the fabric to prepare the electromagnetic shielding fabric.
In patent CN106835712A, polyaniline is deposited on the surface of the fabric, and then ferrite is compounded by using a resin coating reinforcement method, so as to obtain the electromagnetic shielding fabric.
In patent CN109736079A, carbon nanotubes are grafted on the surface of cotton fabric, and then nickel-phosphorus alloy is chemically plated on the surface of the cotton fabric to obtain the electromagnetic shielding fabric.
Patent CN110195351A, preparing multi-wall carbon nano tube/copper sulfide composite coating electromagnetic shielding fabric by using polyacrylonitrile solution.
The drawbacks of the prior art described above are as follows: for example, in patent CN109267199A, the carbon nanofiber bundle is wrapped with polyaniline and then twisted to form a composite material, and the polyaniline-coated carbon nanofiber bundle is difficult to be produced continuously to further form a fabric.
As for polyaniline conductive yarn used in chinese patent CN104810734A, polyaniline, which is a raw material of conductive polymer, has poor conductivity under neutral and alkaline conditions because of its own structure. And the yarn is processed and then woven, so that the workload is large, and the method is not suitable for batch production. The method in patent CN105742474B utilizes cell pulverization, which effectively improves the dispersion performance of carbon nanotubes, but also reduces the length of carbon nanotubes, which is not favorable for the formation of conductive network; in the aniline polymerization process, one part of the polyaniline can coat carbon nano tubes, and the other part of the polyaniline is polymerized in an aqueous solution, but the polyaniline is difficult to dissolve, and formed solid particles are deposited on the surface of the fabric by virtue of physical adsorption and van der Waals force, so that the bonding force with the fabric is weak.
As shown in patent CN102153862B, the polyaniline/carbon nanotube composite electromagnetic shielding composite material is prepared by a suction filtration method, and because the contact resistance between polyaniline-wrapped carbon nanotubes in the suction filtration composite material is large, the conductivity of the polyaniline-wrapped carbon nanotubes is limited, the finally obtained electromagnetic shielding effectiveness is not more than 7dB, and a certain difference is still obtained from the commercial 20dB requirement.
Disclosure of Invention
The invention aims to provide a polyaniline-coated carbon nanotube coating flexible electromagnetic shielding fabric and a preparation method thereof, which are used for solving the problems in the prior art and improving the conductivity and the electromagnetic shielding performance of the fabric.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a preparation method of a polyaniline-coated carbon nanotube coating flexible electromagnetic shielding fabric, which comprises the steps of coating a carboxylated carbon nanotube on the surface of a pretreated fabric, polymerizing aniline on the surface of the fabric in situ, and coating the carbon nanotube with polyaniline to obtain the polyaniline-coated carbon nanotube coating flexible electromagnetic shielding fabric.
Further, the fabrics include cellulose fiber-based fabrics, chemical fiber fabrics and wool fabrics; the pretreatment of the fabric employs different pretreatment methods according to the type of the fabric.
Further, the cellulose fiber fabrics comprise cotton, hemp and regenerated cellulose fabrics; the pretreatment method of the cellulose fiber fabric comprises the following steps: soaking the cellulose fiber fabric in hot alkali solution, washing to be neutral, and drying.
Further, the chemical fiber fabric comprises terylene, acrylic fiber and polypropylene fiber fabric; the pretreatment method of the chemical fiber fabric comprises the following steps: the chemical fabric is washed by acetone and ethanol, dried and then treated by plasma to enhance the surface activity.
Further, the pretreatment method of the wool fabric comprises the following steps: the wool fabric is washed with acetone and ethanol and then soaked in acid.
Further, the carboxylation treatment of the carbon nanotube comprises:
refluxing carbon nano tubes in mixed acid, cooling, diluting with distilled water, carrying out suction filtration, soaking and pickling filter residues, carrying out suction filtration to remove acid liquor, repeatedly washing with deionized water and ethanol to neutrality, carrying out suction filtration and drying for later use, adding the dried carbon nano tubes into a sodium dodecyl benzene sulfonate solution to ensure that the concentration of the carbon nano tubes is 1-10mg/m L and the concentration of the sodium dodecyl benzene sulfonate is 10-20mg/m L, and carrying out ultrasonic dispersion to obtain the carbon nano tube dispersion liquid.
Further, the coating process comprises the following steps: and (3) putting the fabric into the carbon nano tube dispersion liquid, wherein the mass ratio of the carbon nano tube dispersion liquid to the fabric is 50:1, and carrying out magnetic stirring reaction.
Further, after the coating is finished, taking the fabric out of the carbon nano tube dispersion liquid, putting the fabric into HCl-doped aniline solution, slowly dropwise adding an oxidant solution, after the reaction is finished, taking the fabric out, and washing and drying the fabric.
Further, the concentration of the aniline solution is 0.2-2 mol/L, the amount of doped HCl is 3 wt%, the concentration of the oxidant solution is 0.4-2 mol/L, and the oxidant solution is ammonium persulfate or ferric oxide solution and is doped with 5 wt% HCl.
The invention also provides the polyaniline-coated carbon nanotube coating flexible electromagnetic shielding fabric prepared by the preparation method.
According to the invention, a carbon nano tube subjected to carboxylation treatment is coated on the surface of a fabric, then aniline is polymerized in situ on the surface of the fabric, and polyaniline is used for coating the carbon nano tube, so that the polyaniline-coated carbon nano tube coated fabric is obtained. The carboxyl treatment of the carbon nano tube improves the acting force between the fabric and the carbon nano tube, and the coating of the polyaniline not only fills the defects generated by the carboxyl treatment of the carbon nano tube, is beneficial to improving the conductivity of the coated fabric, but also further solves the problem of're-agglomeration' of the carbon nano tube on the surface of the fabric. The carboxylated carbon nano tube has negative charges, the polyaniline has positive charges, the carboxylated carbon nano tube and the polyaniline can be tightly fused through electrostatic interaction force, and meanwhile, a large number of hydrogen bonds and van der Waals force exist between the polyaniline and the fabric, so that the acting force between the polyaniline-coated carbon nano tube coating and the fabric is effectively improved, and the electromagnetic shielding durability is favorably improved. The polyaniline is coated on the surface of the carboxylated carbon nano-coating fabric by an in-situ polymerization method, special equipment is not needed, the process is simple, the cost is low, the production efficiency is high, and the polyaniline can be produced in large scale in the existing textile printing and dyeing equipment; the method solves the double difficulties that polyaniline is difficult to dissolve in organic solvents and the carbon nano tube has poor dispersibility, effectively combines the advantages of polyaniline and the carbon nano tube, and plays a synergistic effect in the aspect of playing excellent electromagnetic shielding performance.
The invention discloses the following technical effects:
1. the flexible fabric is pretreated to a certain degree, oil contamination impurities are removed, the activity of the fabric is increased, and an excellent flexible substrate is provided for the fabric to adsorb the carbon nano tubes and the polyaniline. Meanwhile, the pretreatment enhances the binding force between the fabric and the carbon nano tube and polyaniline, and is beneficial to the durable maintenance of the electromagnetic shielding performance of the coated fabric.
2. The carboxylation treatment of the carbon nano tube improves the dispersibility of the carbon nano tube and the acting force between the carbon nano tube and the fabric, and when aniline is polymerized on the surface of the carbon nano tube in situ, active sites such as carboxyl and the like can be used as polymerization anchor points to make up the defects of the carbon nano tube in the aspect of conductivity; the formed polyaniline wrapping layer further effectively solves the problem of re-agglomeration of the carbon nano tubes.
3. The polyaniline wraps the carbon nano tubes to form a skin-core structure, the skin layer polyaniline effectively absorbs incident electromagnetic waves, the core layer multi-walled carbon nano tubes absorb the electromagnetic waves through skin-core layer interface polarization, the multi-walled carbon nano tubes form an electromagnetic wave reflection and absorption layer with a gradient structure, and the electromagnetic shielding performance of the polyaniline wrapped carbon nano tube coating fabric is effectively improved.
4. When the polyaniline is wrapped on the carbon nanotube coating fabric, no special adhesive is needed, and the method belongs to clean and green production. For the flexible fabric, no adhesive exists, the adhesion phenomenon between fibers and between yarns in the fabric is effectively avoided, so that the flexibility of the fabric is not greatly influenced, and the fabric has a good practical application value.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
Fig. 1 is an SEM image of a polyaniline-coated carbon nanotube coated flexible electromagnetic shielding fabric prepared in example 1 and a control sample thereof, in which (a) raw cotton fiber; (b) polyaniline-coated cotton fibers; (c) carbon nanotube coated cotton fibers; (d) coating cotton fiber with polyaniline-coated carbon nanotube;
fig. 2 is an electrical performance and conductivity graph of the polyaniline-coated carbon nanotube coated flexible electromagnetic shielding fabric and its control sample prepared in example 2, wherein (a) the conductivity graph of the carbon nanotube coated fabric and the polyaniline-coated carbon nanotube coated fabric; (b) carbon nanotube coated fabric, polyaniline coated carbon nanotube coated fabric electromagnetic shielding performance graph;
fig. 3 is a graph showing the influence of the coating times on the flexible electromagnetic shielding fabric coated with the polyaniline-coated carbon nanotube, wherein fig. 3a is a graph showing the influence of the coating times on the electromagnetic shielding performance of the flexible electromagnetic shielding fabric coated with the polyaniline-coated carbon nanotube; 3b is an influence graph of the coating times on the absorption, reflection and transmission of electromagnetic waves of the flexible electromagnetic shielding fabric coated with the polyaniline-coated carbon nanotube;
fig. 4 is a flexible and foldable graph of the polyaniline coated carbon nanotube coated flexible electromagnetic shielding fabric.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
Example 1
Example 1a flexible electromagnetic shielding fabric with a polyaniline-coated carbon nanotube coating was prepared using a cotton woven fabric according to the following steps:
step 1, pretreating cotton machine fabrics, weighing 1L deionized water in a beaker, weighing 20g NaOH, putting the NaOH in the beaker, stirring until the NaOH is dissolved, putting the fabrics in the beaker, soaking the fabrics for 1 hour at a constant temperature of 85 ℃, taking the fabrics out, washing the fabrics to be neutral, and drying the fabrics for later use.
And step 3: putting the pretreated cotton woven fabric into carbon nano tube dispersion liquid, wherein the mass ratio of the carbon nano tube dispersion liquid to the fabric is 50:1, and stirring for 1 hour by using a magnetic stirrer.
And 4, step 4: preparing an aniline monomer solution: preparing 0.8M aniline monomer solution, dripping HCl serving as a doping agent into the aniline monomer solution, taking the fabric obtained in the step 3 out of the carbon nano tube dispersion liquid, and putting the fabric into the prepared aniline monomer solution.
And 5: preparing an oxidant: and (3) preparing 0.8M ammonium persulfate solution, dropwise adding a small amount of hydrochloric acid into the solution, fully stirring the solution, and carrying out ultrasonic treatment for 10min to obtain fully and uniformly mixed ammonium persulfate oxidant solution for later use.
Step 6: and (3) slowly dripping the oxidant solution into the aniline monomer solution soaked with the fabric in the step (4), reacting for 2 hours, taking out the fabric, washing the fabric for multiple times by using deionized water to remove floating solid particles, and drying at 80 ℃.
And 7: repeat step 2-6 2 times.
Example 2
Example 2 the same fabric samples as used in example 1, except for the process step parameters, were prepared as follows:
step 1, pretreating cotton woven fabric, weighing 1L deionized water in a beaker, weighing 20g NaOH, putting the NaOH in the beaker, stirring until the NaOH is dissolved, putting the cotton woven fabric in the beaker, soaking the cotton woven fabric for 1 hour at a constant temperature of 85 ℃, taking the cotton woven fabric out, washing the cotton woven fabric to be neutral, and drying the cotton woven fabric for later use.
And step 3: putting the pretreated cotton woven fabric into carbon nano tube dispersion liquid, wherein the mass ratio of the carbon nano tube dispersion liquid to the fabric is 50:1, and stirring for 1 hour by using a magnetic stirrer.
And 4, step 4: preparing an aniline monomer solution: preparing 0.8M aniline monomer solution, dripping HCl serving as a doping agent into the aniline monomer solution, taking the fabric obtained in the step 3 out of the carbon nano tube dispersion liquid, and putting the fabric into the prepared aniline monomer solution.
And 5: preparing an oxidant: and (3) preparing 0.8M ammonium persulfate solution, dropwise adding a small amount of hydrochloric acid into the solution, fully stirring the solution, and carrying out ultrasonic treatment for 10min to obtain fully and uniformly mixed ammonium persulfate oxidant solution for later use.
Step 6: and (3) slowly dripping the oxidant solution into the aniline monomer solution soaked with the fabric in the step (4), reacting for 2 hours, taking out the fabric, washing the fabric for multiple times by using deionized water to remove floating solid particles, and drying at 80 ℃.
And 7: repeat step 2-6 5 times.
Example 3
The method of the embodiment 3 is the same as that of the embodiment 1, and is different in the adopted fabric, the embodiment 3 adopts the polyester fabric, and the specific method of the embodiment comprises the following steps:
step 1: pretreating the polyester fabric, washing the polyester fabric with acetone and ethanol for 15min, removing oil contamination impurities on the surface of the fabric, drying, and treating with normal pressure plasma for 1min to increase the surface activity of the chemical fiber.
And step 3: and (3) putting the pretreated fabric into the carbon nano tube dispersion liquid, wherein the mass ratio of the carbon nano tube dispersion liquid to the fabric is 50:1, and stirring for 1 hour by using a magnetic stirrer.
And 4, step 4: preparing an aniline monomer solution: preparing 0.8M aniline monomer solution, dripping HCl serving as a doping agent into the aniline monomer solution, taking the fabric out of the carbon nano tube dispersion liquid, and putting the fabric into the prepared aniline monomer solution.
And 5: preparing an oxidant: and (3) preparing 0.8M ammonium persulfate solution, dropwise adding a small amount of hydrochloric acid into the solution, fully stirring the solution, and carrying out ultrasonic treatment for 10min to obtain a fully and uniformly mixed ammonium persulfate oxidant for later use.
Step 6: and (3) slowly dripping the oxidant into the aniline monomer solution soaked with the fabric in the step (4), reacting for 2 hours, taking out the fabric, washing the fabric for multiple times by using deionized water to remove floating solid particles, and drying at 80 ℃.
And 7: repeat step 2-6 2 times.
Example 4
Example 4 is the same as example 1 in terms of the selected method steps, except that the adopted fabric is different, example 4 adopts a wool fabric, and the specific method steps of the example are as follows:
step 1: the wool fabric is washed with acetone and ethanol for 15min, and then soaked with 1M hydrochloric acid for 15min to make the surface of the wool fabric positively charged.
And step 3: and (3) putting the pretreated fabric into the carbon nano tube dispersion liquid, wherein the mass ratio of the carbon nano tube dispersion liquid to the fabric is 50:1, and stirring for 1 hour by using a magnetic stirrer.
And 4, step 4: preparing an aniline monomer solution: preparing 0.8M aniline monomer solution, dripping HCl serving as a doping agent into the monomer solution, taking the fabric out of the carbon nano tube dispersion liquid, and putting the fabric into the prepared aniline monomer solution.
And 5: preparing an oxidant: and (3) preparing 0.8M ammonium persulfate solution, dropwise adding a small amount of hydrochloric acid into the solution, fully stirring the solution, and carrying out ultrasonic treatment for 10min to obtain fully and uniformly mixed ammonium persulfate oxidant solution for later use.
Step 6: and (3) slowly dripping the oxidant solution into the aniline monomer solution soaked with the fabric in the step (4), reacting for 2 hours, taking out the fabric, washing the fabric for multiple times by using deionized water to remove floating solid particles, and drying at 80 ℃.
And 7: repeat step 2-6 2 times.
Example 5
Example 5 the same fabric as used in example 1, except that the selection of the method steps is different, the specific method steps of this example are as follows:
step 1, pretreating cotton machine fabrics, weighing 1L deionized water in a beaker, weighing 20g NaOH, putting the NaOH in the beaker, stirring until the NaOH is dissolved, putting the fabrics in the beaker, soaking the fabrics for 1 hour at a constant temperature of 85 ℃, taking the fabrics out, washing the fabrics to be neutral, and drying the fabrics for later use.
And step 3: putting the pretreated cotton woven fabric into carbon nano tube dispersion liquid, wherein the mass ratio of the carbon nano tube dispersion liquid to the fabric is 50:1, and stirring for 1 hour by using a magnetic stirrer.
And 4, step 4: preparing an aniline monomer solution: preparing 0.8M aniline monomer solution, dripping HCl serving as a doping agent into the aniline monomer solution, taking the fabric obtained in the step 3 out of the carbon nano tube dispersion liquid, and putting the fabric into the prepared aniline monomer solution.
And 5: preparing an oxidant: and (3) preparing 0.8M ammonium persulfate solution, dropwise adding a small amount of hydrochloric acid into the solution, fully stirring the solution, and carrying out ultrasonic treatment for 10min to obtain fully and uniformly mixed ammonium persulfate oxidant solution for later use.
Step 6: and (3) slowly dripping the oxidant solution into the aniline monomer solution soaked with the fabric in the step (4), reacting for 2 hours, taking out the fabric, washing the fabric for multiple times by using deionized water to remove floating solid particles, and drying at 80 ℃.
And 7: repeat step 2-6 2 times.
Example 6
Example 6 the same fabric samples as those selected in example 1 were selected, except that the parameters of the process steps were different, and the specific process steps of this example were as follows:
step 1, pretreating cotton machine fabrics, weighing 1L deionized water in a beaker, weighing 20g NaOH, putting the NaOH in the beaker, stirring until the NaOH is dissolved, putting the fabrics in the beaker, soaking the fabrics for 1 hour at a constant temperature of 85 ℃, taking the fabrics out, washing the fabrics to be neutral, and drying the fabrics for later use.
Step 2: carboxylation treatment of multi-wall carbon nano-tubes: putting the multi-walled carbon nano-tube into mixed acid (the volume ratio of concentrated sulfuric acid to concentrated nitric acid is 3:1), refluxing and stirring for 90min at 95 ℃, then cooling to room temperature, diluting with distilled water, performing suction filtration, putting into washing liquor for soaking and pickling, performing suction filtration to remove pickling liquor after pickling for 1h, repeatedly washing with deionized water and absolute ethyl alcohol until the pH value is 7, performing suction filtration, and drying at 60 ℃ by using a vacuum oven for later use. Weighing a certain amount of carboxylated multi-wall carbon nano-tubes, dispersing the multi-wall carbon nano-tubes (4mg/ml) by using sodium dodecyl benzene sulfonate (10mg/ml), further increasing the dispersibility of the multi-wall carbon nano-tubes by ultrasonic treatment (1h), and preparing a carbon nano-tube dispersion liquid with the concentration of 1 mg/ml.
And step 3: and (3) putting the cleaned fabric into the carbon nano tube dispersion liquid, wherein the mass ratio of the carbon nano tube dispersion liquid to the fabric is 50:1, and stirring for 1 hour by using a magnetic stirrer.
And 4, step 4: preparing an aniline monomer solution: preparing 0.4M aniline monomer solution, dripping HCl serving as a doping agent into the aniline monomer solution, taking the fabric out of the carbon nano tube dispersion liquid, and putting the fabric into the prepared aniline monomer solution.
And 5: preparing an oxidant: and (3) preparing 0.4M ammonium persulfate solution, dropwise adding a small amount of hydrochloric acid into the solution, fully stirring the solution, and carrying out ultrasonic treatment for 10min to obtain fully and uniformly mixed ammonium persulfate oxidant solution for later use.
Step 6: and (3) slowly dripping the oxidant solution into the aniline monomer solution soaked with the fabric in the step (4), reacting for 2 hours, taking out the fabric, washing the fabric for multiple times by using deionized water to remove floating solid particles, and drying at 80 ℃.
And 7: repeat step 2-6 2 times.
Example 7
Example 7 the same fabric as used in example 3, except for the process step parameters, the specific process steps for this example were as follows:
step 1: pretreating the polyester fabric, washing the polyester fabric with acetone and ethanol for 15min, removing oil contamination impurities on the surface of the fabric, drying, and treating with normal pressure plasma for 1min to increase the surface activity of the chemical fiber.
And step 3: and (3) putting the cleaned fabric into the carbon nano tube dispersion liquid, wherein the mass ratio of the carbon nano tube dispersion liquid to the fabric is 50:1, and stirring for 1 hour by using a magnetic stirrer.
And 4, step 4: preparing an aniline monomer solution: preparing 0.8M aniline monomer solution, dripping HCl serving as a doping agent into the aniline monomer solution, taking the fabric out of the carbon nano tube dispersion liquid, and putting the fabric into the prepared aniline monomer solution.
And 5: preparing an oxidant: preparing 0.8M ferric chloride solution, dropwise adding a small amount of hydrochloric acid, fully stirring, and performing ultrasonic treatment for 10min to obtain fully and uniformly mixed ferric chloride oxidant solution for later use.
Step 6: and (3) slowly dripping the oxidant solution into the aniline monomer solution soaked with the fabric in the step (4), reacting for 2 hours, taking out the fabric, washing the fabric for multiple times by using deionized water to remove floating solid particles, and drying at 80 ℃.
And 7: repeat step 2-6 2 times.
To test the various properties of the invention, the following experiments were performed:
1. SEM examination of fabric micro morphology
The polyaniline-coated carbon nanotube-coated fabric prepared in example 1 was used as a sample for SEM scanning to obtain a microscopic morphology, and the results are shown in fig. 1. In order to verify the wrapping of the carbon nanotubes by polyaniline, fabrics only coated with the carbon nanotubes and only coated with the polyaniline were prepared according to example 1, as shown in fig. 1a, raw cotton fibers were relatively smooth, and after the polyaniline coating, the polyaniline coating was observed on the fiber surface, as shown in fig. 1b, and after the carbon nanotube coating, the fiber surface was covered with the carbon nanotube coating, as shown in fig. 1 c; after aniline was polymerized in situ on the surface of the carbon nanotube coated fabric, a layer of polyaniline-wrapped carbon nanotube coating was present on the fiber surface, as shown in fig. 1 d.
2. Influence of polyaniline-coated carbon nanotube coating on electrical property and electromagnetic shielding property of fabric
In order to confirm that the polyaniline-coated carbon nanotube coated fabric has good electrical and conductive properties, fabrics coated with only carbon nanotubes and polyaniline were prepared according to example 2, respectively, and the electrical and electromagnetic shielding properties of the three were compared, with the results shown in fig. 2. As can be seen from fig. 2a, the fabric coated with carbon nanotubes alone does not illuminate the small bulb, while the fabric coated with polyaniline reportedly can illuminate the small bulb. When the small bulb is connected with the polyaniline-coated fabric, the lamp is not lit. This fully indicates that the coating of the carbon nanotubes with polyaniline improves the electrical conductivity of the single component. Comparing the electromagnetic shielding performance of three samples as shown in fig. 2b, the electromagnetic shielding effectiveness of the polyaniline-coated carbon nanotube coated fabric exceeds 20dB, which achieves commercial value, while the electromagnetic shielding effectiveness of the other two samples is less than 8 dB. This further illustrates that the coating of the carbon nanotubes with polyaniline improves the electromagnetic shielding effectiveness of its single component.
3. Influence of coating times on electromagnetic shielding performance of polyaniline-coated carbon nanotube coated fabric
Fabrics with different coating times were obtained by varying the number of repetitions in step 7 according to example 1, and their electromagnetic shielding properties were investigated, as shown in fig. 3 a. It was found that the electromagnetic shielding effectiveness of the coated fabric increased with the number of coatings. Meanwhile, the shielding mechanism is analyzed, and the absorption rate of the polyaniline-coated carbon nanotube coated fabric to electromagnetic waves is more than 50%, and the reflectivity is always less than 50%, which shows that the absorption is the main shielding mechanism, and the reflection is the second, as shown in fig. 3 b.
4. Soft foldability of polyaniline-coated carbon nanotube coated fabric
The bending stiffness of the fabric can represent the softness and comfort of the fabric, and according to example 1, fabrics with different coating times are obtained by changing the times of repeated operation in step 7, and the bending stiffness of the fabrics is studied, as shown in fig. 4, it can be seen that polyaniline-coated carbon nanotube coated fabrics have the same good flexibility as raw cotton and carbon nanotube coated cotton. It was found that the bending stiffness of the coated fabric increased with increasing number of coatings. However, it is still within the comfort range of fabric wear. Therefore, the method for coating the carbon nano tube coating by the polyaniline can prepare the flexible and efficient electromagnetic shielding fabric without the auxiliary action of any adhesive.
In conclusion, different pretreatment is adopted for different fabrics, so that the fabrics have better activity and are convenient for coating finishing of the fabrics. The carbon nano tube is subjected to carboxylation treatment by using the mixed solution of concentrated sulfuric acid and concentrated nitric acid, so that the acting force between the carbon nano tube and the fabric is enhanced, the coating amount of the carbon nano tube on the surface of the fabric is increased, polyaniline is introduced to coat the carbon nano tube, the structural defect of the carbon nano tube at the carboxyl position is overcome, the reunion problem of the carbon nano tube is improved, and the conductivity and the electromagnetic shielding performance of the coated fabric are effectively improved. The whole coating process does not use any adhesive, the flexibility of the fabric is kept, and the flexible electromagnetic shielding fabric has good application prospect in the field of flexible electromagnetic shielding fabrics.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (10)
1. A preparation method of a polyaniline-coated carbon nanotube coating flexible electromagnetic shielding fabric is characterized in that a carbon nanotube subjected to carboxylation treatment is coated on the surface of a pretreated fabric, and then aniline is polymerized on the surface of the fabric in situ to coat the carbon nanotube with polyaniline, so that the polyaniline-coated carbon nanotube coating flexible electromagnetic shielding fabric is obtained.
2. The method according to claim 1, wherein the fabric comprises a cellulose fiber fabric, a chemical fiber fabric or a wool fabric; the pretreatment of the fabric employs different pretreatment methods according to the type of the fabric.
3. The method for preparing the polyaniline coated carbon nanotube coated flexible electromagnetic shielding fabric as claimed in claim 2, wherein the cellulose fiber fabric comprises cotton, hemp, regenerated cellulose fabric; the pretreatment method of the cellulose fiber fabric comprises the following steps: soaking the cellulose fiber fabric in hot alkali solution, washing to be neutral, and drying.
4. The method for preparing the polyaniline-coated carbon nanotube coated flexible electromagnetic shielding fabric as claimed in claim 2, wherein the chemical fiber fabric comprises polyester, acrylic, polypropylene fabric; the pretreatment method of the chemical fiber fabric comprises the following steps: the chemical fabric is washed by acetone and ethanol, dried and then treated by plasma to enhance the surface activity.
5. The method for preparing the polyaniline-coated carbon nanotube coated flexible electromagnetic shielding fabric as claimed in claim 2, wherein the pretreatment method of the wool fabric comprises: the wool fabric is washed with acetone and ethanol and then soaked in acid.
6. The method for preparing the polyaniline-coated carbon nanotube coated flexible electromagnetic shielding fabric as claimed in claim 1, wherein the carboxylation treatment of the carbon nanotubes comprises:
refluxing carbon nano tubes in mixed acid, cooling, diluting with distilled water, carrying out suction filtration, soaking and pickling filter residues, carrying out suction filtration to remove acid liquor, repeatedly washing with deionized water and ethanol to neutrality, carrying out suction filtration and drying for later use, adding the dried carbon nano tubes into a sodium dodecyl benzene sulfonate solution to ensure that the concentration of the carbon nano tubes is 1-10mg/m L and the concentration of the sodium dodecyl benzene sulfonate is 10-20mg/m L, and carrying out ultrasonic dispersion to obtain the carbon nano tube dispersion liquid.
7. The method for preparing the polyaniline-coated carbon nanotube coated flexible electromagnetic shielding fabric as claimed in claim 6, wherein the coating process comprises: and (3) putting the fabric into the carbon nano tube dispersion liquid, wherein the mass ratio of the carbon nano tube dispersion liquid to the fabric is 50:1, and carrying out magnetic stirring reaction.
8. The method for preparing the polyaniline-coated carbon nanotube coated flexible electromagnetic shielding fabric as claimed in claim 7, wherein after the coating is coated, the fabric is taken out of the carbon nanotube dispersion solution, put into the HCl-doped aniline solution, slowly and dropwise added with the oxidant solution, and after the reaction is finished, the fabric is taken out, washed and dried.
9. The method for preparing the polyaniline-coated carbon nanotube coated flexible electromagnetic shielding fabric as claimed in claim 8, wherein the concentration of the aniline solution is 0.2-2 mol/L, the amount of doped HCl is 3 wt%, the concentration of the oxidant solution is 0.4-2 mol/L, and the oxidant solution is ammonium persulfate or ferric oxide solution and is doped with 5 wt% HCl.
10. A polyaniline-coated carbon nanotube-coated flexible electromagnetic shielding fabric prepared by the preparation method of any one of claims 1 to 9.
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