CN109754950B - Preparation method of flexible conductive fabric substrate with low surface roughness - Google Patents

Preparation method of flexible conductive fabric substrate with low surface roughness Download PDF

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CN109754950B
CN109754950B CN201811635972.2A CN201811635972A CN109754950B CN 109754950 B CN109754950 B CN 109754950B CN 201811635972 A CN201811635972 A CN 201811635972A CN 109754950 B CN109754950 B CN 109754950B
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nano silver
polyvinyl alcohol
fabric
glass slide
silver wire
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CN109754950A (en
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杜平凡
邱琳琳
庄志山
丁明乐
夏广波
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Zhejiang Sci Tech University ZSTU
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Zhejiang Sci Tech University ZSTU
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Abstract

The invention discloses a preparation method of a flexible conductive fabric substrate with low surface roughness. A layer of nano silver wire fiber film is prepared by spin coating on a cleaned glass slide through a demolding process; coating a layer of polyvinyl alcohol aqueous solution on the cloth, and immediately covering the cloth on the cloth; and peeling off the glass slide after drying to prepare the flexible conductive fabric substrate with the structure of cloth-polyvinyl alcohol-nano silver wire fiber from bottom to top. The method has the advantages of simple and repeatable process, easily obtained raw materials and controllable cost, and the prepared flexible conductive fabric has good conductivity and surface smoothness and excellent light transmittance, can be used as a carrier of various flexible energy devices such as fabric-based solar cells and the like, and is widely applied to the field of electronic devices and the field of wearable technology.

Description

Preparation method of flexible conductive fabric substrate with low surface roughness
Technical Field
The invention relates to the field of electronic devices and the preparation of flexible conductive substrates in the field of wearable technology, in particular to a preparation method of a flexible conductive fabric substrate with low surface roughness.
Background
Today, technology is changing day by day, and various electronic devices such as smart phones, AI glasses, and smart watches accompany our daily lives. In the face of the technical surge of electronic products, researchers generally think that the wearable intelligent fabric prepared by miniaturizing and flexibilizing some electronic devices and combining the electronic devices with the fabric can better expand the application of the electronic products and enrich the lives of people. The electronic device is directly combined with the fabric, such as outdoor clothes, hats, backpacks, tents and the like, to form the extensible ultra-flexible wearable intelligent textile, so that the weight of the wearable intelligent textile in outdoor activities can be reduced, and the use comfort of the wearable equipment is improved.
However, some intelligent electronic devices such as a novel solar cell and an Organic Light Emitting Diode (OLED) have a very thin film layer, which is only several hundred nanometers or even several tens nanometers thick, so that the problem that a conductive layer is directly formed on a fabric, which has too high surface roughness and does not utilize the growth of the film layer, is encountered, and the development of wearable intelligent textiles is limited. In view of the above, the invention innovatively uses a demolding process, selects a glass slide as a template substrate, and generates a layer of nano silver wire film as a conductive medium by spin coating on the glass slide; then selecting high polymer polyvinyl alcohol as a demoulding high polymer material, coating the high polymer material on a glass slide-nano silver wire fiber substrate, and covering the selected plain weave fabric on a polymer before the high polymer is cured; heating for a period of time, and peeling off the materials to obtain the flexible fabric conductive substrate respectively comprising cloth, polyvinyl alcohol and nano silver wire fibers from bottom to top. The conductive fabric substrate prepared by the method has good light transmission and excellent conductivity, more importantly, has smooth surface and low roughness, and can be applied to large-scale preparation of wearable intelligent devices with higher requirements on the surface roughness of the substrate.
Disclosure of Invention
In order to solve the problems in the background art, the invention provides a preparation method of a flexible conductive fabric substrate with low surface roughness. And (3) by utilizing a demolding process, taking the wave plate as a demolding substrate, spin-coating a layer of nano silver wire solution on the wave plate, then blade-coating a layer of polyvinyl alcohol on the wave plate, covering the wave plate with a fabric, and drying to prepare the flexible conductive fabric substrate with a smooth surface and good conductivity.
The technical scheme adopted by the invention is as follows:
the invention comprises the following steps:
1) cleaning fabrics and glass slides: ultrasonically washing the fabric for 15 minutes by respectively using soap water and alcohol, taking out and drying to obtain the washed fabric, and ultrasonically washing the glass slide for 15 minutes by respectively using soap water, acetone and deionized water to obtain a clean glass slide;
2) and (3) processing the nano silver wire solution: sealing the nano silver wire solution, uniformly shaking, then placing the solution in an ultrasonic cleaning instrument for ultrasonic treatment, and obtaining the treated nano silver wire solution after the nano silver wires are uniformly dispersed in the solvent without generating precipitation;
3) spin coating of a nano silver wire solution: carrying out ultraviolet ozone treatment on the cleaned glass slide in the step 1) for 15 minutes, fixing the glass slide on a suction cup of a spin coating instrument, dropwise adding and spin-coating the nano silver wire solution treated in the step 2) on the surface of the glass slide, and finally placing the glass slide on a heating plate for heating and drying to prepare a sample I;
4) preparing a polyvinyl alcohol (PVA124) solution: adding polyvinyl alcohol powder into deionized water, and placing the mixture into a magnetic water bath kettle to be heated, stirred and dissolved to obtain a polyvinyl alcohol (PVA124) solution.
5) Blade coating of polyvinyl alcohol solution: scraping the polyvinyl alcohol solution obtained in the step 4) on the sample I obtained in the step 3) by using a blade to obtain an undried sample II;
6) covering fabric: flatly laying the fabric cleaned in the step 1) on the sample II which is not dried in the step 5), and drying the fabric on a heating plate to obtain a sample III;
7) uncovering the sample: and (3) after the sample III in the step 6) is cooled, removing the sample III from the glass slide to prepare the flexible conductive fabric substrate.
In the step 2), the ultrasonic treatment is ultrasonic vibration dispersion for 15 minutes by using an ultrasonic cleaning instrument.
In the step 3), the rotating speed of spin coating is 1000-2000 rpm, the spin coating time is 20-40 seconds, the heating temperature on the heating plate is 110-130 ℃, and the heating time is 5-15 minutes.
In the step 4), the mass percentage concentration of the polyvinyl alcohol solution is 5 wt% -15 wt%, the water bath stirring temperature is 90-100 ℃, and the water bath stirring time is 2-4 hours.
In the step 6), the drying temperature of the heating plate is 50-70 ℃, and the drying time is 3-10 minutes.
The invention has the beneficial effects that:
1) the conductive fabric substrate prepared successfully by the method has the advantages of easily available raw materials, controllable cost, simple and repeatable process and strong operability.
2) The surface roughness of the conductive fabric substrate successfully prepared by the method is obviously reduced.
3) The flexible conductive fabric prepared by the invention has good conductivity and surface smoothness and excellent light transmittance, can be used as a carrier of various flexible energy devices such as fabric-based solar cells and the like, and is widely applied to the fields of electronic devices and wearable technologies.
Drawings
Fig. 1 is a schematic flow diagram of the conductive fabric substrate prepared in example 1.
FIG. 2 is a surface topography of the fabric-polyvinyl alcohol film prepared in example 1 (a direct knife coating method, b release method).
FIG. 3 is a surface topography of the fabric-polyvinyl alcohol-silver nanowires prepared in example 1 (a and c are direct blade coating methods, b and d are release methods).
FIG. 4 is a schematic diagram of the bonding mode of polyvinyl alcohol and silver nanowires in the sample prepared in example 1 (a direct knife coating method, b demolding method).
Fig. 5 is a pictorial representation of the conductive fabric substrate prepared in example 1.
FIG. 6 is a surface topography of a conductive fabric substrate prepared by two methods of example 1 after spin coating a perovskite film layer thereon (a direct doctor blading method, b-demolding method).
Fig. 7 is a graph of light transmittance of the conductive fabric substrate, fabric-polyvinyl alcohol, and fabric prepared in example 1.
Detailed Description
The invention is further illustrated by the following figures and examples.
The examples of the invention are as follows:
example 1:
as shown in figure 1, ultrasonically washing the fabric with soap water and alcohol for 15 min, taking out and drying; simultaneously, ultrasonically washing the glass slide for 15 minutes by using soap water, acetone and deionized water respectively; sealing the purchased nano silver wire solution, shaking the nano silver wire solution by hand for several times, and placing the nano silver wire solution in an ultrasonic cleaning instrument to ultrasonically vibrate and disperse the nano silver wire in the nano silver wire solution for 15 minutes so as to uniformly disperse the nano silver wire solution in the solvent without generating precipitates; adding polyvinyl alcohol powder into deionized water, placing the mixture in a magnetic water bath kettle, heating the mixture at 95 ℃, and magnetically stirring the mixture for 3 hours to dissolve the mixture, thereby preparing the polyvinyl alcohol solution with the mass percentage concentration of 10 wt%.
Preparing a conductive fabric substrate by a demolding method: spin-coating the nano silver wire solution on a cleaned glass slide at the spin-coating speed of 1200 rpm for 30 seconds, and then heating at 120 ℃ for 15 minutes; after the conductive fabric substrate is cooled, the prepared polyvinyl alcohol solution is dripped, the uniform-speed knife coating is carried out by using a scalpel, the substrate fabric is immediately laid on the substrate fabric, the substrate fabric is placed on a heating plate, and the substrate fabric is taken off after being heated for 5 minutes at the temperature of 60 ℃ to prepare the conductive fabric substrate.
As a control, a direct knife coating method was also performed to prepare a conductive fabric substrate, and related data were also measured.
As shown in fig. 2, which is a surface topography diagram of the fabric-polyvinyl alcohol film prepared in example 1, fig. 2(a) adopts the direct doctor-blading method, and fig. 2(b) adopts the demolding method of the present invention, it can be found that the fabric-polyvinyl alcohol film prepared by the present invention has a flat surface without the surface relief phenomenon of the film prepared by the direct doctor-blading method.
As shown in fig. 3, which is a surface topography diagram of the fabric-polyvinyl alcohol-silver nanowires prepared in example 1, fig. 3(a) and 3(c) adopt a direct blade coating method, and fig. 3(b) and 3(d) adopt a demolding method of the present invention, the silver nanowires of the substrate prepared by the method of the present invention are uniformly distributed, and the phenomenon of uneven coating does not occur.
As shown in fig. 4, which is a schematic view of the combination mode of the polyvinyl alcohol and the nano silver wire of the sample prepared in example 1, fig. 4(a) adopts a direct blade coating method, and fig. 4(b) adopts the demolding method of the present invention, it can be found that the combination mode of the polyvinyl alcohol film and the nano silver wire is embedded in the polyvinyl alcohol film, which is beneficial to the surface smoothness of the prepared conductive fabric substrate, compared with the direct blade coating method.
As shown in fig. 5, the conductive fabric substrate prepared by the demolding method of the invention in example 1 has good conductivity, and the square resistance value is 35-60 Ω.
As shown in fig. 6, which is a surface topography diagram of the perovskite spin-coated on the conductive fabric substrate prepared by the two methods in example 1, fig. 6(a) adopts a direct blade coating method, fig. 6(b) adopts the demolding method of the present invention, and the perovskite thin film spin-coated on the conductive fabric substrate prepared by the method of the present invention has good topography and uniform distribution; the perovskite spin-coated on the conductive fabric substrate prepared by the direct blade coating method cannot completely cover the substrate, so that the thickness is uneven, and the nano silver wire is exposed.
Fig. 7 is a graph showing the transmittance curves of the conductive fabric substrate, the fabric-polyvinyl alcohol and the fabric prepared by the demolding method of the present invention, and the transmittance of the conductive fabric substrate prepared by the method of the present invention exceeds 50% under most of the wavelength conditions in the visible light range, which indicates that the prepared conductive fabric substrate has good transmittance.
Example 2:
ultrasonically washing the fabric with soap water and alcohol for 15 min, taking out and drying; simultaneously, ultrasonically washing the glass slide for 15 minutes by using soap water, acetone and deionized water respectively; sealing the purchased nano silver wire solution, shaking the nano silver wire solution by hand for several times, and placing the nano silver wire solution in an ultrasonic cleaning instrument to ultrasonically shake and disperse the nano silver wires in the nano silver wire solution for 15 minutes so as to uniformly disperse the nano silver wires in the solvent without generating precipitates; adding polyvinyl alcohol powder into deionized water, placing the mixture in a magnetic water bath kettle, heating the mixture at 90 ℃, and magnetically stirring the mixture for 2 hours to dissolve the mixture, thereby preparing the polyvinyl alcohol solution with the mass percentage concentration of 5 wt%.
Preparing a conductive fabric substrate: spin-coating the nano silver wire solution on a cleaned glass slide at the speed of 1000 rpm for 20 seconds, and then heating at 110 ℃ for 5 minutes; after the conductive fabric substrate is cooled, the prepared polyvinyl alcohol solution is dripped, the uniform-speed knife coating is carried out by using a scalpel, the substrate fabric is immediately laid on the substrate fabric, the substrate fabric is placed on a heating plate, and the substrate fabric is taken off after being heated for 3 minutes at 50 ℃ to prepare the conductive fabric substrate.
The flow chart, the fabric-polyvinyl alcohol surface appearance graph, the nano silver wire distribution electron microscope photo, the material object graph, the square resistance value, the perovskite spin coating surface appearance graph, the light transmittance curve graph and the like of the sample prepared in the embodiment are similar to those of the embodiment 1.
Example 3:
ultrasonically washing the fabric with soap water and alcohol for 15 min, taking out and drying; simultaneously, ultrasonically washing the glass slide for 15 minutes by using soap water, acetone and deionized water respectively; sealing the purchased nano silver wire solution, shaking the nano silver wire solution by hand for several times, and placing the nano silver wire solution in an ultrasonic cleaning instrument to ultrasonically shake and disperse the nano silver wires in the nano silver wire solution for 15 minutes so as to uniformly disperse the nano silver wires in the solvent without generating precipitates; adding polyvinyl alcohol powder into deionized water, placing the mixture into a magnetic water bath kettle, heating the mixture at 100 ℃, and magnetically stirring the mixture for 4 hours to dissolve the mixture, thereby preparing the polyvinyl alcohol solution with the mass percentage concentration of 15 wt%.
Preparing a conductive fabric substrate: spin-coating the nano silver wire solution on a cleaned slide, wherein the spin-coating speed is 2000 rpm for 40 seconds, and then heating the slide at 130 ℃ for 15 minutes; after the conductive fabric substrate is cooled, the prepared polyvinyl alcohol solution is dripped, the uniform-speed knife coating is carried out by using a scalpel, the substrate fabric is immediately laid on the substrate fabric, the substrate fabric is placed on a heating plate, the substrate fabric is heated at 70 ℃ for 10 minutes and then is taken off, and the conductive fabric substrate is prepared.
The flow chart, the fabric-polyvinyl alcohol surface appearance graph, the nano silver wire distribution electron microscope photo, the material object graph, the square resistance value, the perovskite spin coating surface appearance graph, the light transmittance curve graph and the like of the sample prepared in the embodiment are similar to those of the embodiment 1.

Claims (2)

1. A method for preparing a flexible conductive fabric substrate with low surface roughness is characterized in that,
the method comprises the following steps:
1) cleaning fabrics and glass slides: ultrasonically washing the fabric for 15 minutes by respectively using soap water and alcohol, taking out and drying to obtain the washed fabric, and ultrasonically washing the glass slide for 15 minutes by respectively using soap water, acetone and deionized water to obtain a clean glass slide;
2) and (3) processing the nano silver wire solution: sealing the nano silver wire solution, uniformly shaking, then placing the solution in an ultrasonic cleaning instrument for ultrasonic treatment, and obtaining the treated nano silver wire solution after the nano silver wires are uniformly dispersed in the solvent without generating precipitation;
3) spin coating of a nano silver wire solution: carrying out ultraviolet ozone treatment on the cleaned glass slide in the step 1) for 15 minutes, fixing the glass slide on a suction cup of a spin coating instrument, dropwise adding and spin-coating the nano silver wire solution treated in the step 2) on the surface of the glass slide, and finally placing the glass slide on a heating plate for heating and drying to prepare a sample I;
in the step 3), the rotation speed of spin coating is 1000-2000 rpm, the spin coating time is 20-40 seconds, the heating temperature on the heating plate is 110-130 ℃, and the heating time is 5-15 minutes;
4) preparing a polyvinyl alcohol solution: adding polyvinyl alcohol powder into deionized water, and placing the mixture into a magnetic water bath kettle to be heated, stirred and dissolved to obtain a polyvinyl alcohol solution;
in the step 4), the mass percentage concentration of the polyvinyl alcohol solution is 5 wt% -15 wt%, the water bath stirring temperature is 90-100 ℃, and the water bath stirring time is 2-4 hours;
5) blade coating of polyvinyl alcohol solution: scraping the polyvinyl alcohol solution obtained in the step 4) on the sample I obtained in the step 3) by using a blade to obtain an undried sample II;
6) covering fabric: flatly laying the fabric cleaned in the step 1) on the sample II which is not dried in the step 5), and drying the fabric on a heating plate to obtain a sample III;
in the step 6), the drying temperature of the heating plate is 50-70 ℃, and the drying time is 3-10 minutes;
7) uncovering the sample: and (3) after the sample III in the step 6) is cooled, removing the sample III from the glass slide to prepare the flexible conductive fabric substrate.
2. The method of claim 1, wherein the flexible conductive fabric substrate with low surface roughness is prepared by the following steps: in the step 2), the ultrasonic treatment is ultrasonic vibration dispersion for 15 minutes by using an ultrasonic cleaning instrument.
CN201811635972.2A 2018-12-29 2018-12-29 Preparation method of flexible conductive fabric substrate with low surface roughness Active CN109754950B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103762014A (en) * 2013-12-24 2014-04-30 苏州大学 Flexible and transparent electrode film based on silk fibroin and manufacturing method and application thereof
CN104637570A (en) * 2015-01-29 2015-05-20 深圳市东丽华科技有限公司 Flexible transparent conductive thin film and preparation method thereof
CN108221368A (en) * 2017-12-15 2018-06-29 华南理工大学 A kind of conductive fabric and preparation method thereof
CN108648854A (en) * 2018-05-10 2018-10-12 佛山市瑞福物联科技有限公司 A kind of nano-silver thread conductive structure and preparation method thereof for wearable device
CN109077713A (en) * 2018-07-23 2018-12-25 华中科技大学 A kind of preparation method of human epidermal physiological electrode sensor

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8703235B2 (en) * 2007-02-23 2014-04-22 The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration Preparation of metal nanowire decorated carbon allotropes

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103762014A (en) * 2013-12-24 2014-04-30 苏州大学 Flexible and transparent electrode film based on silk fibroin and manufacturing method and application thereof
CN104637570A (en) * 2015-01-29 2015-05-20 深圳市东丽华科技有限公司 Flexible transparent conductive thin film and preparation method thereof
CN108221368A (en) * 2017-12-15 2018-06-29 华南理工大学 A kind of conductive fabric and preparation method thereof
CN108648854A (en) * 2018-05-10 2018-10-12 佛山市瑞福物联科技有限公司 A kind of nano-silver thread conductive structure and preparation method thereof for wearable device
CN109077713A (en) * 2018-07-23 2018-12-25 华中科技大学 A kind of preparation method of human epidermal physiological electrode sensor

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