KR102605564B1 - Method for producing conductive fiber, and fiber manufactured by using the same - Google Patents

Abstract

One embodiment of the present invention includes preparing a coating solution containing a carbon-conductive polymer composite in which carbon quantum dots are dispersed in a conductive polymer; and forming a conductive coating layer on the fiber by immersing the fiber in the coating solution, wherein the carbon quantum dots add thermal stability to the conductive fiber manufacturing method and the conductive fiber manufactured thereby with improved electrical properties and thermal stability. to provide.

Description

Manufacturing method of conductive fiber and conductive fiber manufactured according to the manufacturing method {METHOD FOR PRODUCING CONDUCTIVE FIBER, AND FIBER MANUFACTURED BY USING THE SAME}

The present invention relates to conductive fibers, and more specifically, to a method of manufacturing conductive fibers with improved electrical properties and thermal stability by coating the fibers with a coating solution in which carbon quantum dots are dispersed in a conductive polymer.

[R&D project that supported this invention]

[Assignment identification number] JA-21-0001

[Ministry name] Government contribution

[Research Management Institute] Korea Institute of Industrial Technology

[Research project name] Corporate demand-based production technology commercialization project (5/5)

[Research project name] [Integrated EZ] Development of highly functional source material technology for smart textronics

[Contribution rate] 30%

[Host research institute] Korea Institute of Industrial Technology

Conductive fibers serve as an important element of wearable devices and functional fibers, and are also used in various fields, including as sensors. Therefore, attempts are being made to apply various materials.

Looking at each material before this, metal-based materials have the advantage of excellent conductivity, but they have the fatal disadvantage that the resistance value changes significantly as the temperature changes, and there is a possibility of oxidation if left in the air for a long time, shortening the lifespan. The downside is that it is not long. In addition, due to the nature of functional fibers that must be in direct contact with the skin, the stability problem caused by metal in direct contact with the skin has not been resolved.

Next, nanocarbon-based materials are likely to be suitable for functional fibers because they are highly stable and low in toxicity enough to allow contact with the skin. However, it has the disadvantage of being difficult to introduce uniformly due to its lack of adsorption with fibers, so it is not suitable for application to conductive fibers.

Additionally, the materials being attempted are conductive polymers such as polyacetylene, polypyrrole, polythiophene, and PEDOT (poly(3,4-ethylenedioxythiophene)). Conductive polymers have excellent electrical conductivity, have characteristics of stability and less toxicity than metal-based materials, and have excellent adsorption with fibers, so they have the advantage of being able to produce uniform conductive fibers. However, conductive polymers have a fatal drawback in that their resistance value changes rapidly depending on temperature changes. In this way, if the resistance value of conductive fiber changes depending on temperature, it cannot be used in various environments, so conductive polymers also have distinct limitations as a material for conductive fibers. Therefore, there is a need for the development of conductive fibers that can be applied to various devices with excellent electrical properties and thermal stability as essential conditions.

(Patent) Republic of Korea Patent No. 10-2016-0033856

The technical problem to be achieved by the present invention is to provide a method of producing a conductive fiber with improved electrical properties and thermal stability by preparing a coating solution and immersing the fiber in the coating solution.

Another embodiment of the present invention provides a conductive fiber with improved electrical properties and thermal stability manufactured by the above manufacturing method.

The technical problem to be achieved by the present invention is not limited to the technical problem mentioned above, and other technical problems not mentioned can be clearly understood by those skilled in the art from the description below. There will be.

In order to achieve the above technical problem, an embodiment of the present invention provides a method for manufacturing conductive fiber.

In an embodiment of the present invention, a method for manufacturing a conductive fiber includes preparing a coating solution containing a carbon-conductive polymer composite in which carbon quantum dots are dispersed in a conductive polymer; and immersing the fiber in the coating solution to form a conductive coating layer on the fiber, and the carbon quantum dots may be a method of manufacturing a conductive fiber with improved electrical properties and thermal stability by adding thermal stability.

At this time, the carbon quantum dots dispersed in the conductive polymer may modify the morphology of the conductive polymer to reduce the interface resistance of the carbon-conductive polymer composite.

Additionally, in this case, the conductive polymer may include poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate)(PEDOT:PSS).

Additionally, at this time, the carbon quantum dots may have a size of 2 nm to 4 nm.

Additionally, at this time, the carbon quantum dots may be characterized as carbon quantum dots into which a metal is introduced.

Additionally, at this time, the metal may be characterized as including a transition metal.

Additionally, in this case, the transition metal may include nickel or silver.

In addition, at this time, the metal-introduced carbon quantum dots include step (a) of preparing a metal precursor solution by mixing the metal precursor with distilled water; Then, step (b) of mixing and stirring the solution of step (a) and the carbon precursor; Then, step (c) of hydrothermally synthesizing the solution of step (b); Afterwards, step (d) of cooling the solution of step (c); Afterwards, step (e) of filtering the solution of step (d) through a filter and then washing it; And it may be characterized in that it is manufactured in step (f) of drying the solution of step (e).

Additionally, at this time, the carbon precursor in step (b) may be characterized as containing fumaronitrile (C ₄ H ₂ N ₂ ).

In addition, at this time, forming a conductive coating layer on the fiber includes the step (g) of converting the surface to hydrophilicity by treating the surface of the fiber with oxygen plasma as a pretreatment; And it may further include step (h) of adding and mixing additives to improve coating ability in the coating solution.

In addition, at this time, the additive in step (h) may be a conductive fiber manufacturing method characterized in that it contains dimethyl sulfoxide (DMSO) and 4-dodecylbenzenesulfonic acid.

In order to achieve the above technical problem, another embodiment of the present invention provides a conductive fiber.

In an embodiment of the present invention, the conductive fiber is a fiber; And it may be a conductive fiber characterized by improved electrical properties and thermal stability, including a conductive coating layer located on the fiber and including a carbon-conductive polymer composite in which carbon quantum dots are dispersed in a conductive polymer.

At this time, the carbon quantum dots dispersed in the conductive polymer may modify the morphology of the conductive polymer to reduce the interface resistance of the carbon-conductive polymer composite.

Additionally, at this time, the conductive polymer may be characterized as containing poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate)(PEDOT:PSS).

Additionally, at this time, the carbon quantum dots may have a size of 2 nm to 4 nm.

Additionally, at this time, the carbon quantum dots may be characterized as carbon quantum dots into which a metal is introduced.

Additionally, at this time, the metal may be characterized as including a transition metal.

Additionally, in this case, the transition metal may be a conductive fiber characterized in that it contains nickel or silver.

According to an embodiment of the present invention, the steps of preparing a coating solution containing a carbon-conductive polymer composite in which carbon quantum dots introduced with a transition metal are dispersed in a conductive polymer and immersing a fiber in the coating solution to form a conductive coating layer on the fiber A method for manufacturing a conductive fiber with improved electrical properties and thermal stability can be provided, including the step of: and a conductive fiber according to the manufacturing method can be provided.

Accordingly, by compensating for the disadvantages of metal-based materials and conductive polymer-based materials and combining their advantages, it is possible to manufacture a universally usable conductive fiber that overcomes changes in resistance value depending on temperature and shows consistent electrical properties at various temperatures. .

The effects of the present invention are not limited to the effects described above, and should be understood to include all effects that can be inferred from the configuration of the invention described in the detailed description or claims of the present invention.

Figure 1 is a schematic diagram of a carbon-conductive polymer composite and a conductive fiber coated with the composite.
Figure 2 is a schematic diagram of a method for manufacturing a conductive fiber according to an embodiment of the present invention.
Figure 3 is (a) a transmission electron micrograph, (b) a size distribution graph, and (c) a transmission electron micrograph observing the lattice size of carbon quantum dots of a conductive fiber, which is an embodiment of the present invention.
Figure 4 shows (a) Fourier transform infrared spectral data of carbon quantum dots, (b) ultraviolet-visible spectral data by concentration of carbon quantum dots, and (c) excitation of carbon quantum dots for carbon quantum dots of a conductive fiber, which is an embodiment of the present invention. These are photoluminescence data by wavelength, (d) photoexcitation data by emission wavelength of carbon quantum dots, (ef) X-ray photoelectron spectroscopy data of carbon quantum dots.
Figure 5 shows (a) X-ray photoelectron spectroscopy data, (b) ultraviolet-visible photoelectron spectroscopy data, and (cd) atomic force microscopy data for the conductive polymer and carbon-conductive polymer composite of the conductive fiber, which is an embodiment of the present invention. am.
Figure 6 shows resistance change data according to temperature of a conductive fiber containing a carbon-conductive polymer composite in an embodiment of the present invention.
Figure 7 shows resistance change data according to temperature of a conductive fiber containing a carbon-conductive polymer composite into which Ag is introduced as a metal in the conductive fiber according to an embodiment of the present invention.
Figure 8 shows resistance change data according to temperature of a conductive fiber containing a carbon-conductive polymer composite into which Ni is introduced as a metal in the conductive fiber according to an embodiment of the present invention.

Hereinafter, the present invention will be described with reference to the attached drawings. However, the present invention may be implemented in various different forms and, therefore, is not limited to the embodiments described herein. In order to clearly explain the present invention in the drawings, parts that are not related to the description are omitted, and similar parts are given similar reference numerals throughout the specification.

Throughout the specification, when a part is said to be "connected (connected, contacted, combined)" with another part, this means not only "directly connected" but also "indirectly connected" with another member in between. "Includes cases where it is. In addition, when a part is said to “include” a certain component, this does not mean that other components are excluded, but that other components can be added, unless specifically stated to the contrary.

The terms used herein are only used to describe specific embodiments and are not intended to limit the invention. Singular expressions include plural expressions unless the context clearly dictates otherwise. In this specification, terms such as “comprise” or “have” are intended to indicate the presence of features, numbers, steps, operations, components, parts, or combinations thereof described in the specification, but are not intended to indicate the presence of one or more other features. It should be understood that this does not exclude in advance the possibility of the existence or addition of elements, numbers, steps, operations, components, parts, or combinations thereof.

Hereinafter, embodiments of the present invention will be described in detail with reference to the attached drawings.

1 and 2, FIG. 1(a) is a schematic diagram of a carbon-conductive polymer composite 300 of conductive fiber 400, which is an embodiment of the present invention, and FIG. 1(b) is an embodiment of the present invention. This is a schematic diagram of the conductive fiber 400. Figure 2 is a schematic diagram of a manufacturing method of the conductive fiber 400, which is an embodiment of the present invention.

Looking at the manufacturing method of the conductive fiber 400, which is an embodiment of the present invention, with reference to Figure 1, the manufacturing method of the conductive fiber 400 is a carbon-conductive polymer composite in which carbon quantum dots 100 are dispersed in a conductive polymer 200. Preparing a coating solution containing (300); and immersing the fiber in the coating solution to form a conductive coating layer on the fiber, wherein the carbon quantum dots 100 add thermal stability, thereby producing a conductive fiber 400 with improved electrical properties and thermal stability. It is characterized by

At this time, the carbon quantum dots 100 dispersed in the conductive polymer 200 are characterized in that they reduce the interface resistance of the carbon-conductive polymer composite 300 by modifying the morphology of the conductive polymer 200.

Looking specifically, the currently commonly used conductive polymer (200) has the advantage of excellent electrical properties and adhesion to fibers, but has the fatal disadvantage of rapidly changing electrical properties as the temperature changes, and the conductive polymer (200) based on carbon quantum dots (100) Although the material has excellent electrical properties and thermal stability. It has the disadvantage of not adhering well to fibers. Therefore, in order to compensate for the shortcomings and maximize the advantages through the present invention, based on the carbon quantum dots (100), the carbon quantum dots (100) are introduced in a form in which the carbon quantum dots (100) are evenly dispersed in the conductive polymer (200) to improve electrical conductivity and carbon quantum dots (100) ) is intended to formulate a special structure that also utilizes thermal stability. Through this, the goal is to secure competitiveness by improving electrical properties and stably securing electrical properties in response to temperature changes, while improving thermal stability and manufacturing a new conductive fiber 400 through improved morphology.

Looking at each material, the conductive polymer 200 may be a conductive polymer 200 such as polyacetylene, polypyrrole, polythiophene, poly(3,4-ethylenedioxythiophene) (PEDOT), etc. . However, it is not limited thereto, and a person skilled in the art of the present invention will know that, like the above-mentioned materials, they have excellent electrical conductivity, are less stable and less toxic than metal-based materials, and have excellent adsorption with fibers, resulting in uniform conductivity. Materials that can be used to fabricate fiber 400 should be construed as falling within the scope of the present invention. In the present invention, in particular, an embodiment was implemented including poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate) (PEDOT:PSS) as the conductive polymer 200 material. In the case of PEDOT:PSS, the carbon quantum dots 100 It is introduced and dispersed in PEDOT:PSS, and upon introduction, the carbon quantum dot (100) aqueous solution acts as a polar solvent and replaces PSS, which is an electrical insulator, thereby reducing the specific gravity of PSS in PEDOT:PSS. Accordingly, the reduction of PSS, which plays a role in aggregating PEDOT in PEDOT:PSS, reduces the agglomeration of the carbon-conductive polymer composite 300, and a morphological change occurs in which the size of the particles increases, resulting in a decrease in resistance at the interface and at the same time electrical By reducing PSS, which is an insulator, and increasing carbon quantum dots (100) with excellent electrical properties and thermal stability, a carbon-conductive polymer composite (300) with improved electrical conductivity while maintaining thermal stability is formed.

Looking at carbon quantum dots (100) as the next material, carbon quantum dots (100), a type of nanocarbon, are nanoscale carbon composites and have optical and surface electronic properties due to non-covalent bonds due to pi-pi stacking between carbon composites. In addition, the zero-dimensional carbon quantum dots (100) manufactured according to the method for manufacturing the conductive fiber (400), which is an embodiment of the present invention, are composed of covalent bonds within the nanoscale carbon composite, so they are thermally very stable and the carbon quantum dots (100) ) is nanoscale, so unlike other carbon-based materials, it has very abundant functional groups, and the functional groups serve as active edge sites and have excellent electrical properties.

Next, looking at the carbon-conductive polymer composite 300 containing the conductive polymer 200 and the carbon quantum dots 100 and the coating solution containing the same, it was formulated through the carbon quantum dots 100 and the conductive polymer 200. Even in the case of the carbon-conductive polymer composite 300, the material properties of the carbon quantum dots 100 and the conductive polymer 200 can be maintained. Accordingly, the manufactured carbon-conductive polymer composite 300 has electrical properties and thermal stability due to the carbon quantum dots 100, and it can be expected that it can be used at various temperatures by minimizing the change in resistance value depending on temperature.

Next, referring to FIG. 3, in the method of manufacturing the conductive fiber 400, which is an embodiment of the present invention, and the conductive fiber 400 manufactured thereby, the carbon quantum dots 100 are preferably 2 nm to 4 nm in size. do. Specifically, in the case of quantum dots, the optical properties vary greatly depending on the size, so a size of 2 nm to 4 nm is preferable for formulation with the conductive polymer targeted by the present invention, and the above range also varies depending on the size as previously discussed. Because uniform size means uniform characteristics of these changing quantum dots, it is important to control them within the narrow size range described above. According to Figure 3 (a), it can be seen that the carbon quantum dots 100 are evenly dispersed within the conductive polymer 200, and according to Figures 3 (b) and (c), as mentioned above, carbon quantum dots ( It can be seen that most 100) are manufactured to have a size of 2 nm to 3 nm.

Next, in the method of manufacturing the conductive fiber 400 and the conductive fiber 400 manufactured according to the method according to an embodiment of the present invention, the carbon quantum dots 100 may be carbon quantum dots 100 into which a metal is introduced, and the metal is a transition material. May contain metal. Additionally, the transition metal may include nickel or silver. Specifically, in order to improve the electrical properties of the conductive fiber 400, various transition metals such as nickel or silver are introduced into the carbon quantum dots 100. In addition to improving the electrical properties, if other properties are to be improved, It is also possible to introduce non-metallic elements such as nitrogen and phosphorus. Therefore, the materials that can be introduced into the carbon quantum dots 100 are not limited to the materials mentioned above, and include materials that can be easily used by those skilled in the art to improve the properties of the carbon-conductive polymer. It should be interpreted as including all.

Next, looking specifically in terms of the manufacturing method, in the method of manufacturing the conductive fiber 400, which is an embodiment of the present invention, and the conductive fiber 400 manufactured thereby, the carbon quantum dots 100 into which the metal is introduced are prepared by replacing the metal precursor with distilled water. Step (a) of preparing a metal precursor solution by mixing with; Then, step (b) of mixing and stirring the solution of step (a) and the carbon precursor; Then, step (c) of hydrothermally synthesizing the solution of step (b); Afterwards, step (d) of cooling the solution of step (c); Afterwards, step (e) of filtering the solution of step (d) through a filter and then washing it; And then it is characterized in that it is prepared by step (f) of drying the solution of step (e). Specific experimental conditions will be examined in the experimental examples below.

Next, in the method of manufacturing the conductive fiber 400, which is an embodiment of the present invention, the step of forming a conductive coating layer on the fiber is step (g) of converting the surface to hydrophilicity by treating the surface of the fiber with oxygen plasma as a pretreatment. ; And it may further include step (h) of adding and mixing additives to improve coating ability into the coating solution. Likewise, specific experimental conditions will be examined in the experimental examples below.

Next, the conductive fiber 400 manufactured according to the method for manufacturing the conductive fiber 400, which is an embodiment of the present invention, will be described.

Referring to Figure 1, which was previously examined, the conductive fiber 400 is a fiber; And a conductive coating layer located on the fiber and including a carbon-conductive polymer composite 300 in which carbon quantum dots 100 are dispersed within the conductive polymer 200, and is characterized by improved electrical properties and thermal stability.

At this time, the carbon quantum dots 100 dispersed in the conductive polymer 200 are characterized in that they reduce the interface resistance of the carbon-conductive polymer composite 300 by modifying the morphology of the conductive polymer 200.

Additionally, at this time, the conductive polymer 200 may include poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate)(PEDOT:PSS).

Additionally, at this time, the carbon quantum dots 100 may be carbon quantum dots 100 into which a metal is introduced, and the metal may include a transition metal. Additionally, the transition metal may include nickel or silver. However, it is not limited thereto and should be construed to include materials that can be easily used by those skilled in the art to improve the electrical properties of the carbon-conductive polymer composite 300.

Next, the carbon quantum dots 100 preferably have a size of 2 nm to 4 nm, as previously discussed in the manufacturing method of the conductive fiber 400. Specifically, in the case of quantum dots, the optical properties vary greatly depending on the size, so a size of 2 nm to 4 nm is preferable for formulation with the conductive polymer targeted by the present invention, and the above range also varies depending on the size as previously discussed. Because uniform size means uniform characteristics of these changing quantum dots, it is important to control them within the narrow size range described above.

Since the description of the carbon quantum dots 100, the conductive polymer 200, and the carbon-conductive polymer composite 300 is the same as the manufacturing method of the conductive fiber 400 discussed above, repeated descriptions will be omitted.

Next, looking at the possibility of utilizing the conductive fiber 400, which is an embodiment of the present invention, the main purpose is to formulate a conductive polymer 200 incorporating carbon quantum dots 100 to overcome the change in resistance value depending on temperature and to It is a manufacturing of conductive fiber 400 that shows consistent electrical properties and can be used for general purposes. Based on this, it is expected to be applied to functional fibers and sensors, or to be used in various fields such as wearable devices.

Example 1

Method for manufacturing carbon quantum dots with transition metals introduced

1. Step (a)

This is the step of preparing a transition metal precursor solution by mixing the transition metal precursor with distilled water. In detail in this example, the transition metal precursor is prepared by dissolving 0.21 g of silver nitrate or 0.22 g of nickel acetate in 100 ml of distilled water.

2. Step (b)

Thereafter, step (b) involves mixing the solution of step (a) with the carbon precursor and stirring it.

3 ml of the transition metal precursor aqueous solution prepared through step (a) above is stirred at 150 rpm for 30 minutes with 300 mg of Fumaronitrile (C ₄ H ₂ N ₂ ) corresponding to the carbon precursor.

3. Step (c)

Afterwards, the solution of step (b) is hydrothermally synthesized. Specifically, the solution obtained through stirring in step (b) is placed in a Teflon liner and then assembled again in a high-pressure sterilization device (Autoclave). Immerse the assembled autoclave device in a water bath containing silicone oil preheated to 200 degrees. Hydrothermal synthesis was performed in the silicone oil bath while stirring at 150 rpm for 15 minutes.

4. Step (d)

Afterwards, the solution of step (c) is cooled. Specifically, after the hydrothermal synthesis is completed, the high-pressure sterilization device is cooled in cold water for 15 minutes. After additional cooling is completed, dismantle the assembled high-pressure sterilization device, open the Teflon liner, and add an additional 9 ml of distilled water. Then, stir at 400 rpm for 5 minutes using a stirrer.

5. Step (e)

Afterwards, the solution in step (d) is filtered through a filter and then washed. Specifically, after stirring, the obtained solution is filtered using a PTFE membrane as a filter, sufficiently dispersed using distilled water and ethanol as a solvent, and then washed through centrifugation several times to remove residual salt by-products.

6. Step (f)

Afterwards, the solution of step (e) is dried. Specifically, the final solution is stored in an ultra-low temperature freezer at -80°C for 1 hour and then freeze-dried for 3 days to produce carbon quantum dots in powder form with transition metals introduced.

Example 2

Method for producing a coating solution containing a carbon-conductive polymer composite using carbon quantum dots into which the transition metal is introduced

In this example, there are several types of conductive polymers, but among them, poly (3,4-ethylenedioxythiophene) polystyrene sulfonate (PEDOT:PSS) was used.

Specifically, 8 mg of carbon quantum dots containing nickel or silver in powder form were added to 1 mL of PEDOT:PSS diluted to a concentration of 3% in water, and then dispersed for 30 minutes using an ultrasonicator for uniform dispersion.

Through this, a solution containing a carbon-conductive polymer composite in which carbon quantum dots with a transition metal introduced into the conductive polymer are uniformly dispersed is produced. The prepared solution has a structure in which carbon quantum dots with about 2 nm to 3 nm of transition metal introduced are evenly dispersed between the conductive polymers. Through this special structure, the particle size of the conductive polymer can be increased as mentioned above. As a result, the resistance occurring at the interface between existing conductive polymer particles is minimized to improve electrical properties, and at the same time, by using the characteristics of the conductive polymer, carbon quantum dots, which previously lack adsorption with fibers, can be uniformly introduced.

In addition, it not only improves the electrical properties by improving the morphology of existing conductive polymers, but also improves the surface functional groups of carbon quantum dots such as hydroxyl group (-OH), pyridinic-N, pyrrolic-N, and graphene. Graphitic-N can further increase conductivity.

Example 3

Method of forming a conductive coating layer on the fiber with the coating solution

A step of forming a conductive coating layer on the fiber by immersing the fiber in the coating solution. In this case, the step of forming a conductive coating layer on the fiber involves treating the surface of the fiber with oxygen plasma as a pretreatment to convert the surface to hydrophilicity. Step (g); and

It is characterized in that it further includes step (h) of adding and mixing additives to improve coating ability in the coating solution.

1. Step (g)

This is the step of converting the surface to hydrophilicity by surface treating the fiber with oxygen plasma.

In this example, the fiber uses spandex, and the spandex is treated through an oxygen plasma processor for 5 minutes to change the surface to hydrophilicity and improve coating ability.

2. Step (h)

This is the step of adding and mixing additives to improve coating ability in the coating solution. Specifically, to improve the coating ability of the fiber, 0.5 g of DMSO (Dimethyl Sulfoxide) and 0.1 g of 4-dodecylbenzenesulfonic acid were added to 1 mL of the coating solution (PEDOT:PSS+Ni CQD powder) prepared according to Example 2, and then added for 20 minutes. Disperse using an ultrasonic cleaner.

3. Method of coating fibers with the above coating solution

The spandex treated in step (g) is added to the coating solution prepared in step (h) and treated in an ultrasonic cleaner for 15 minutes. Afterwards, the fibers are taken out and dried at room temperature for 40 minutes. Afterwards, the dried fiber is further dried in an oven at a temperature of 120°C for 20 minutes. Thereafter, the above method can be repeated a total of three times to produce a fiber coated with a carbon-conductive polymer composite into which a transition metal is introduced.

Experimental Example 1

Experiment to measure the properties of carbon quantum dots manufactured according to the conductive fiber manufacturing method, which is an embodiment of the present invention

Figure 4 shows (a) Fourier transform infrared spectral data of carbon quantum dots, (b) ultraviolet-visible spectral data by concentration of carbon quantum dots, and (c) excitation of carbon quantum dots for carbon quantum dots of a conductive fiber, which is an embodiment of the present invention. These are photoluminescence data by wavelength, (d) photoexcitation data by emission wavelength of carbon quantum dots, (e-f) X-ray photoelectron spectroscopy data of carbon quantum dots.

Experimental Example 2

Experiment to measure the properties of a carbon-conductive polymer composite manufactured according to the conductive fiber manufacturing method, which is an embodiment of the present invention

Figure 5 shows (a) X-ray photoelectron spectroscopy data, (b) ultraviolet-visible photoelectron spectroscopy data, and (c-d) atomic force microscopy data for the conductive polymer and carbon-conductive polymer composite of the conductive fiber, which is an embodiment of the present invention. am.

According to Figure 5(a), in the case of carbon-conductive polymer composite (N-CQD in PEDOT:PSS), the intensity of PEDOT is confirmed to be increased compared to the conductive polymer (PEDOT:PSS) in which carbon quantum dots are not introduced. This means that with the introduction of carbon quantum dots, PSS was replaced by carbon quantum dots within the conductive polymer and the proportion of PEDOT within the resulting conductive polymer increased. Through this, as explained earlier, the proportion of PSS, which is an electrical insulator, is reduced, and carbon quantum dots with excellent electrical properties are introduced, so that the electrical properties of the carbon-conductive polymer composite are improved compared to the conductive polymer without carbon quantum dots. You can expect it to become excellent.

According to Figure 5(b), in the case of carbon-conductive polymer composite (N-CQD in PEDOT:PSS), it is confirmed that the binding energy is reduced compared to the conductive polymer (PEDOT:PSS) in which carbon quantum dots are not introduced. It can be expected that with the introduction of carbon quantum dots, the morphology of the conductive polymer was modified and the particle size increased. In addition, as previously explained, as the particle size increases, the resistance generated at the interface decreases, which can be expected to improve electrical properties.

Experimental Example 3

Experiment to measure electrical properties of conductive fibers manufactured according to the conductive fiber manufacturing method, which is an embodiment of the present invention

This will be described with reference to FIGS. 6 to 8.

Figure 6 shows resistance change data according to temperature of a conductive fiber containing a carbon-conductive polymer composite in an embodiment of the present invention.

Figure 7 shows resistance change data according to temperature of a conductive fiber containing a carbon-conductive polymer composite into which Ag is introduced as a metal in the conductive fiber according to an embodiment of the present invention.

Figure 8 shows resistance change data according to temperature of a conductive fiber containing a carbon-conductive polymer composite into which Ni is introduced as a metal in the conductive fiber according to an embodiment of the present invention.

The above data was measured using a Provestation, and specifically, the fiber was fixed on a slide glass with copper tape and then applied silver paste to measure the resistance value.

According to the above data, the conductive fiber without carbon quantum dots had a resistance value of 53307 Ω/cm at 25°C, and the resistance decreased significantly as the temperature increased. On the other hand, in the case of conductive fibers into which carbon quantum dots were introduced, when PEDOT:PSS and N-CQD were mixed at a volume ratio of 3:6, resistance was 1548 Ω/cm at 25°C, and in the case of conductive fibers without carbon quantum dots, In comparison, it was confirmed that the change in resistance as the temperature increased was relatively small. Likewise, when mixed with Ag-CQD at a 3:6 volume ratio, the resistance was 1738 Ω/cm at 25℃, and in the case of Ni-CQD, when mixed with PEDOT:PSS at a 3:6 volume ratio, the resistance was 2176 Ω/cm at 25℃. It was confirmed that the change in resistance with increase in temperature was relatively small compared to the case of the conductive fiber in which the carbon quantum dots were not introduced.

Experimental Example 4

Experiment to measure the thermal stability of conductive fibers manufactured according to the conductive fiber manufacturing method, which is an embodiment of the present invention

Description will be made with reference to FIGS. 6 to 8.

Figure 6 shows resistance change data according to temperature of a conductive fiber containing a carbon-conductive polymer composite in an embodiment of the present invention.

Figure 7 shows resistance change data according to temperature of a conductive fiber containing a carbon-conductive polymer composite into which Ag is introduced as a metal in the conductive fiber according to an embodiment of the present invention.

Figure 8 shows resistance change data according to temperature of a conductive fiber containing a carbon-conductive polymer composite into which Ni is introduced as a metal in the conductive fiber according to an embodiment of the present invention.

The data was measured by placing the manufactured conductive fiber sample in a drying oven, setting the starting temperature to 25°C, and measuring the resistance value every time the temperature increased by 5°C.

According to the data above, in the case of conductive fibers without carbon quantum dots, a 51% change in resistance value occurred when the temperature changed from 25℃ to 80℃, 19% in the case of N-CQD, and 18% in the case of Ag-CQD. %, in the case of Ni-CQD, a resistance change of 20% was measured. Therefore, compared to conductive fibers without carbon quantum dots, the thermal resistance stability was confirmed to be 2.68 times improved for N-CQDs, 2.83 times for Ag-CQDs, and 2.55 times for Ni-CQDs.

The description of the present invention described above is for illustrative purposes, and those skilled in the art will understand that the present invention can be easily modified into other specific forms without changing the technical idea or essential features of the present invention. will be. Therefore, the embodiments described above should be understood in all respects as illustrative and not restrictive. For example, each component described as unitary may be implemented in a distributed manner, and similarly, components described as distributed may also be implemented in a combined form.

The scope of the present invention is indicated by the patent claims described below, and all changes or modified forms derived from the meaning and scope of the claims and their equivalent concepts should be construed as being included in the scope of the present invention.

100: carbon quantum dot
200: Conductive polymer
300: Carbon-conductive polymer composite
400: conductive fiber

Claims (18)

Preparing a coating solution containing a carbon-conductive polymer composite in which carbon quantum dots are dispersed in a conductive polymer; and
Comprising the step of immersing a fiber in the coating solution to form a conductive coating layer on the fiber,
The carbon quantum dots add thermal stability, improving electrical properties and thermal stability,
The carbon quantum dot is a carbon quantum dot into which a metal is introduced, and the metal includes a transition metal. According to paragraph 1,
The carbon quantum dots dispersed in the conductive polymer modify the morphology of the conductive polymer to reduce the interface resistance of the carbon-conductive polymer composite. According to paragraph 1,
A method of producing a conductive fiber, wherein the conductive polymer includes poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate)(PEDOT:PSS). According to paragraph 1,
A method of manufacturing a conductive fiber, characterized in that the carbon quantum dots have a size of 2 nm to 4 nm. delete delete According to paragraph 1,
A method of manufacturing a conductive fiber, characterized in that the transition metal includes nickel or silver. According to paragraph 1,
The carbon quantum dots into which the metal is introduced are
Step (a) of preparing a metal precursor solution by mixing the metal precursor with distilled water;
Then, step (b) of mixing and stirring the solution of step (a) and the carbon precursor;
Then, step (c) of hydrothermally synthesizing the solution of step (b);
Afterwards, step (d) of cooling the solution of step (c);
Afterwards, step (e) of filtering the solution of step (d) through a filter and then washing it; and
A method of producing a conductive fiber, characterized in that it is manufactured in step (f) of drying the solution of step (e). According to clause 8,
The carbon precursor in step (b) is a conductive fiber manufacturing method, characterized in that it contains fumaronitrile (C ₄ H ₂ N ₂ ). According to paragraph 1,
The step of forming a conductive coating layer on the fiber is pretreatment.
Step (g) of converting the surface to hydrophilicity by treating the surface of the fiber with oxygen plasma; and
A method of producing a conductive fiber, further comprising the step (h) of adding and mixing an additive to improve coating ability in the coating solution. According to clause 10,
The additive in step (h) includes dimethyl sulfoxide (DMSO) and 4-dodecylbenzenesulfonic acid. fiber; and
A conductive coating layer located on the fiber and including a carbon-conductive polymer composite in which carbon quantum dots are dispersed in a conductive polymer,
Electrical properties and thermal stability are improved,
The carbon quantum dots are carbon quantum dots into which a metal is introduced, and the metal includes a transition metal. According to clause 12,
The carbon quantum dots dispersed in the conductive polymer modify the morphology of the conductive polymer to reduce the interface resistance of the carbon-conductive polymer composite. According to clause 12,
A conductive fiber characterized in that the conductive polymer includes poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate)(PEDOT:PSS). According to clause 12,
A conductive fiber characterized in that the carbon quantum dots have a size of 2 nm to 4 nm. delete delete According to clause 12,
A conductive fiber characterized in that the transition metal includes nickel or silver.