KR101790707B1 - Conductive master batch and method for manufacturing thereof and method for manufacturing conductive film using the same - Google Patents
Conductive master batch and method for manufacturing thereof and method for manufacturing conductive film using the same Download PDFInfo
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- KR101790707B1 KR101790707B1 KR1020150046380A KR20150046380A KR101790707B1 KR 101790707 B1 KR101790707 B1 KR 101790707B1 KR 1020150046380 A KR1020150046380 A KR 1020150046380A KR 20150046380 A KR20150046380 A KR 20150046380A KR 101790707 B1 KR101790707 B1 KR 101790707B1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0023—Apparatus or processes specially adapted for manufacturing conductors or cables for welding together plastic insulated wires side-by-side
Abstract
The present invention relates to a conductive masterbatch in which carbon nanotubes are mixed, a method of manufacturing the conductive masterbatch, and a method of manufacturing a conductive film using the conductive masterbatch. In particular, a method of manufacturing a conductive film according to an embodiment of the present invention includes: Preparing; Preparing a synthetic resin base material for producing a film; mixing the master batch with the synthetic resin base material; and extruding the synthetic base material mixed with the master batch to produce a film.
Description
The present invention relates to a conductive masterbatch having a small surface resistance and improved dispersibility, a method for producing the conductive masterbatch, and a method for producing a conductive film using the masterbatch.
In general, the transparent conductive film is used for a plasma display panel (PDP), a liquid crystal display (LCD) device, a light emitting diode device (LED), an organic electroluminescence device (OLEL), a touch panel or a solar cell.
The most common method for producing such a transparent conductive film is a method of mixing various materials having conductivity with a dispersion and applying the mixture to the surface of a transparent film.
On the other hand, a material that has been recently spotlighted as a conductive material is carbon nanotubes (CNTs). Carbon nanotubes are graphite sheets that have a nano-sized diameter and are rolled into a tubular shape. The diameter of the tube is in the range of a few nanometers to a few tens of nanometers. Carbon nanotubes are known as new materials with excellent mechanical properties, electrical conductivity and thermal conductivity, excellent field emission characteristics, and high efficiency hydrogen storage media characteristics.
However, as far as the marketability of carbon nanotubes is concerned, all focus has been limited to the manufacture of liquid dispersions and film coating methods.
As for the method of applying general carbon nanotubes to a nonconductive base material, a method of producing a transparent conductive film containing carbon nanotubes and a binder and a transparent conductive film (manufactured by the same) A method for manufacturing a nanotube coating film and a method for manufacturing a carbon nanotube-coated film (Japanese Patent Application Laid-Open No. 10-0050566).
For example, in the case of producing a conductive film, carbon nanotubes are dispersed in a volatile organic compound (VOC), which is an organic solvent, to prepare a coating solution. Then, the coating solution is coated on the surface of the film, Or coating with a binder. Therefore, the process is complicated and costly, and the coating film is easily peeled off from the base material of the film depending on the use of the film.
Particularly, carbon nanotubes are not easily aggregated and dispersed in a solution, and when one component is added to a pure solution, the conductivity is deteriorated and carbon nanotube stabilization is easily broken, so that the solution does not become a uniform solution but is easily aggregated.
Therefore, recently, it is time to demand a technique that can easily handle carbon nanotubes that are difficult to handle and simplify the process of manufacturing a conductive film.
Accordingly, the inventor of the present invention has developed a technology to utilize a carbon nanotube in a completely new manner by completely removing the coating technique of the carbon nanotube if the carbon nanotube can be processed in the master batch used for plastic processing and added to all the plastic film forming And suggested this technology.
It is an object of the present invention to provide a conductive master batch comprising a carbon nanotube and a conductive silicone polymer that is complementary in dispersibility of carbon nanotubes and capable of controlling the surface resistance value.
It is still another object of the present invention to provide a method for producing a carbon nanotube, which comprises mixing carbon nanotubes and toluene, mixing a mixture of the carbon nanotubes and toluene with a conductive silicone polymer, and mixing the carbon nanotubes and the conductive silicone polymer using an extruder And processing the mixture into a pellet form.
A conductive masterbatch according to an embodiment of the present invention includes a carbon nanotube and a conductive silicone polymer.
The conductive silicone polymer may include any conductive filler selected from the group consisting of carbon materials, metals, metal oxides, and combinations thereof.
The weight ratio of the carbon nanotubes to the conductive silicone polymer is preferably 4: 6 to 7: 3.
The conductive silicone polymer is preferably transparent and has a weight average molecular weight falling within the range of 1,000 to 800,000 g / mol.
According to another embodiment of the present invention, there is provided a method of manufacturing a semiconductor device, comprising: mixing a carbon nanotube and a conductive silicone polymer; And processing the mixture of the carbon nanotubes and the conductive silicone polymer into a pellet form by using an extruder.
In the mixing step, the weight ratio of the carbon nanotube to the conductive silicone polymer is preferably 4: 6 to 7: 3.
The conductive silicone polymer preferably has a weight average molecular weight in the range of 1,000 to 800,000 g / mol.
Mixing the carbon nanotubes with a silicon member having a weight average molecular weight in the range of 1,000 to 100,000 g / mol, and mixing the mixture of the carbon nanotubes and the silicon member with the conductive silicone polymer , And the conductive silicone polymer preferably has a weight average molecular weight in the range of 100,000 to 800,000 g / mol.
Or mixing of the carbon nanotubes and the toluene preferably includes mixing the carbon nanotubes and the toluene and mixing the mixture of the carbon nanotubes and the toluene with the conductive silicone polymer.
The mixing of the carbon nanotubes and the toluene may be performed by mixing 80 to 95 wt% of the carbon nanotubes and 5 to 20 wt% of the toluene.
Meanwhile, a method of manufacturing a conductive film according to an embodiment of the present invention includes: preparing a master batch according to the master batch manufacturing method; Preparing a synthetic resin base material for producing a film; Mixing the synthetic resin matrix and the conductive master batch; And forming a film by extrusion-molding the synthetic resin base material mixed with the conductive master batch.
The synthetic resin base material is preferably one or more of low density polyethylene (LDPE), polyethylene terephthalate (PET), polyvinyl chloride (PVC), and thermoplastic polyurethane (TPU).
In the step of mixing the master batch with the synthetic resin base material, it is preferable that the master batch is mixed with 1 to 20 wt% and the synthetic resin base material is mixed with 80 to 99 wt%.
According to the embodiment of the present invention, the conductive silicon polymer is impregnated with carbon nanotubes having excellent conductivity to prepare a master batch in the form of a pellet, and by directly extruding the conductive film using the master batch, The conductive film can be produced in a new way out of the way of coating the conductive material incorporated in various dispersions on the surface of the film during production.
In addition, toluene is added to the conductive master batch at a certain ratio to stabilize the dispersion, and a film having a desired thickness can be produced.
Thus, the effect of improving the production process, manufacturing cost, and production efficiency of the conductive film can be expected. In addition, it is possible to prevent the phenomenon that the film and the conductive material coated on its surface are peeled off as in the prior art.
In addition, the carbon nanotubes can be directly impregnated into the film during the production of the conductive film, and the same or lower surface resistance value can be obtained by including more carbon nanotubes in comparison with the product in which the carbon nanotubes are coated on the surface of the film There is an effect that can be obtained.
In addition, there is an effect that carbon nanotubes can be easily handled by using a polymeric material which is harmless to the human body and is environment-friendly.
Hereinafter, embodiments of the present invention will be described in more detail. It will be apparent to those skilled in the art that the present invention may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, It is provided to let you know.
First, the conductive masterbatch according to an embodiment of the present invention is formed by mixing carbon nanotubes with a conductive silicone polymer.
The polysiloxane, which is the main chain of the silicone polymer, exhibits good insulating properties, and the silica, which is the main filler, is also an insulating material, so that the silicone polymer is mostly used as an insulating material. However, this material having excellent characteristics and processability can be imparted with conductivity and its use can be improved. As a means of conducting the silicon polymer, a conductive filler is used. As the conductive filler, carbon materials such as graphite and carbon black, metals such as silver and nickel, and metal oxides such as silica and alumina may be used. The conductive silicone polymer may have various forms such as one-component type, two-component type, condensation type, and addition type depending on the application, and may be used selectively in consideration of the conductive property. The optimum resistivity of the conductive silicone polymer may be in the range of (1/10) 3 to 10 3 Ω · m.
The conductive silicone polymer is a high molecular weight polymer having a weight average molecular weight of 1,000 to 800,000 g / mol, and has a physical property that viscosity increases as the weight average molecular weight becomes larger. Such a conductive silicone polymer is expected to have an effect of easily handling carbon nanotubes that are environmentally friendly and harmless to the human body and are relatively difficult to handle, as compared with conventional dispersions.
On the other hand, the carbon nanotube (CNT) is a material which imparts conductivity to a film as it is impregnated into a film during the production of a film by mixing with a conductive silicone polymer. Hexagons having six carbon atoms are connected to each other to form a tube As a new material, the tube diameter is only a few to several tens of nanometers. Especially, the electrical conductivity is excellent enough to be similar to copper.
The conductive silicone polymer and the carbon nanotube are mixed to prepare a master batch for producing a film, wherein the weight ratio of the conductive silicone polymer to the carbon nanotube may be 4: 6 to 7: 3. In particular, in order to lower the surface resistance value and increase the dispersibility, it is most preferable that the mixing ratio of the conductive silicone polymer and the carbon nanotube is in the ratio of 5: 5 by weight to less than 7: 3 by weight based on the carbon nanotube.
It is expected that the greater the amount of carbon nanotubes mixed in the conductive silicone polymer, the better the conductivity. However, the reason for limiting the mixing amount of the carbon nanotubes as described above is that when the conductive silicone polymer is mixed with the carbon nanotubes, So that the carbon nanotubes can be sufficiently uniformly mixed with the conductive silicone polymer while the temperature rises due to the self-friction heat during mixing.
The present invention relates to a method of manufacturing a conductive master cell, comprising the steps of mixing a carbon nanotube and a conductive liquid silicone polymer, and processing the mixture of the carbon nanotube and the conductive liquid silicone polymer into a pellet form by using an extruder. A batch manufacturing method is provided.
In the mixing step, the weight ratio of the carbon nanotube to the conductive silicone polymer is preferably 4: 6 to 7: 3, and the conductive silicone polymer has a weight average molecular weight of 1,000 to 800,000 g / mol. .
Before mixing the carbon nanotubes and the conductive silicone polymer, the carbon nanotubes may be first mixed with the silicon member having a weight average molecular weight in the range of 1,000 to 100,000 g / mol. The silicon member has the same characteristics as the conductive silicone polymer described above except for the weight average molecular weight. The mixture of these and the conductive silicone polymer is then mixed. In this case, the weight average molecular weight of the conductive silicone polymer is in the range of 100,000 to 800,000 g / mol.
The reason why the polymer material is divided into the carbon nanotubes in a stepwise manner according to the weight average molecular weight is that the viscosity of the silicon member having a relatively low weight average molecular weight is lower and therefore mixing with the carbon nanotubes is easier. Carbon nanotubes are more dispersed than in a silicon member having a low weight average molecular weight. When the silicon member and the carbon nanotube having a higher viscosity are low and the carbon nanotubes are sufficiently stirred, and then the mixture is stirred with the conductive silicone polymer having a high viscosity, the conductive silicone polymer and the carbon nanotube can be mixed more uniformly.
Alternatively, the liquefierable polymer and the carbon nanotubes can be first mixed, and then the mixture and the conductive silicone polymer can be mixed. The polymer used in this case can be selected from polymers in which the carbon nanotubes are more dispersed than the polymer material. For example, as such a polymer, a polyester polyol or polyethylene having a predetermined viscosity may be used. The polyol is an oligomer state before the production of the resin, and the weight average molecular weight of the initiator and the product is changed in accordance with the intended use.
When mixing the carbon nanotubes and the conductive silicone polymer, the carbon nanotubes and the toluene may be mixed first, and then the mixture of the carbon nanotubes and the toluene mixed with the conductive silicone polymer may be mixed. Toluene allows the mixed carbon nanotubes to be easily mixed with a high molecular weight conductive silicone polymer having a high viscosity. At this time, the toluene is volatilized by the heat generated in the process of mixing the conductive silicon polymer and the carbon nanotube. By adding a certain amount of the toluene, the dispersed CNTs are stabilized and thus the film can be produced to a desired thickness.
The mixing of the carbon nanotubes and the toluene may be performed by mixing 80 to 95 wt% of carbon nanotubes and 5 to 20 wt% of the toluene.
If the toluene is mixed at less than 5 wt%, the carbon nanotubes may not be uniformly dispersed and may aggregate. When the amount of toluene is more than 20 wt%, dispersion instability may occur.
10 to 15 wt% of the toluene is most preferable in terms of dispersion stabilization.
In order to improve the conductivity of the master batch, an additional conductive material may be added and mixed. The conductive material may be selected from a variety of conductive materials such as, for example, silver nanomaterials, magnesium, and the like. Conductive materials can be mixed into the master batch in powder form.
The mixture of the carbon nanotubes and the conductive silicon polymer is processed into a pellet using an extruder. At this time, the size of the pellets is not limited to a specific size, and may be manufactured in various sizes corresponding to extruders for producing a film.
A method of manufacturing a conductive film using the master batch prepared as described above will be described.
First, a master batch containing carbon nanotubes is prepared as described above.
Further, a synthetic resin base material for film production is prepared. At this time, the synthetic resin base material is also preferably prepared in the form of pellets.
As the synthetic resin base material, various kinds of synthetic resins capable of producing a film may be used. For example, as a synthetic resin base material, at least one of low density polyethylene (LDPE), polyethylene terephthalate (PET), polyvinyl chloride (PVC), and thermoplastic polyurethane (TPU), which are representative synthetic resins for producing films, can be used.
Thus, after the master batch is mixed with the synthetic resin base material, the synthetic base resin mixed with the master batch is extruded to produce a film. When extruded, the pellet-shaped master batch is broken, and the carbon nanotubes contained in the pellets can be spread evenly on the synthetic resin base material.
In the step of mixing the master batch with the synthetic resin base material, it is preferable that the master batch is mixed with 1 to 20 wt%, and the synthetic resin base material is mixed with 80 to 99 wt%.
When the masterbatch is contained in an amount less than 1 wt%, the conductivity decreases. When the amount of the masterbatch is more than 20 wt%, there is no difference in the superiority of conductivity, but the production cost increases.
Films prepared from the masterbatch according to the present invention can be used as an electronic protective film or an electrostatic protective film.
[ Example ]
The following examples illustrate the present invention.
First, 6 kg of conductive silicone polymer is administered to a reader capable of processing a plastic master batch, and then 4 Kg of carbon nanotubes is administered to the reader.
Then, the reader is mixed with about 40 minutes at room temperature without heating separately. At this time, the temperature of the conductive silicon polymer and the carbon nanotubes is increased while the heat of the conductive silicon polymer and the carbon nanotubes are generated, and the conductive silicone polymer and the carbon nanotubes are uniformly mixed by the generated heat.
The mixture in which the conductive silicone polymer and the carbon nanotube are mixed is injected into an extruder for master batch processing to prepare a master batch.
The prepared master batch is produced by using a single-layer extruder or a two or more-layer extruder for secondary processing for producing a film.
For example, in the case of using a single-layer extruder, a hopper is produced by applying a synthetic base material and a master batch together. However, in such a case, as carbon nanotubes having a high price are impregnated, the manufacturing cost of the film can be increased.
Therefore, it is economical to use a two-layer extruder rather than a single-layer extruder.
For example, in the case of using a two-layer extruder, only the synthetic resin base material is applied to the first layer hopper, and the master batch and the synthetic resin base material are simultaneously applied to the second layer hopper to produce a film. At this time, the master batch is mixed with 1 to 20 wt%, and the synthetic resin base material is mixed with 80 to 99 wt%.
In order to investigate the utility of the master batch produced in the above manner, various tests were conducted to prepare a film by mixing the various types of synthetic resin base materials while changing the mixing amount of the master batch and measuring the conductivity of the film.
[Experiment 1]
First, a master batch prepared by mixing a conductive silicone polymer and a carbon nanotube at a mixing ratio of 4: 6 by weight was prepared. Then, 10000 g of LDPE was injected into the first layer hopper of the two-layer extruder, 9750 g of LDPE was injected into the second layer hopper, The master batch was changed to 250 g, 750 g, 1250 g, 1750 g, 2500 g, 3750 g and 5000 g in the order of 9250 g, 8750 g, 8250 g, 7500 g, 6250 g and 5000 g in the order of changing the mixing amount of LDPE. And processed into a film.
The thickness of the film thus formed was 40 占 퐉, the thickness of the portion containing carbon nanotubes was 15 占 퐉, and the thickness of the portion where only LDPE was present was 25 占 퐉.
[Experiment 2]
First, a master batch prepared by mixing the conductive silicone polymer and the carbon nanotube in a weight ratio of 5: 5 was prepared. Then, 10000 g of LDPE was injected into the first layer hopper of the two-layer extruder, 9750 g of LDPE was injected into the second layer hopper, The master batch was changed to 250 g, 750 g, 1250 g, 1750 g, 2500 g, 3750 g and 5000 g in the order of 9250 g, 8750 g, 8250 g, 7500 g, 6250 g and 5000 g in the order of changing the mixing amount of LDPE. And processed into a film.
The thickness of the film thus formed was 40 占 퐉, the thickness of the portion containing carbon nanotubes was 15 占 퐉, and the thickness of the portion where only LDPE was present was 25 占 퐉.
[Experiment 3]
First, a master batch prepared by mixing a conductive silicon polymer and a carbon nanotube in a weight ratio of 6: 4 was prepared. Then, 10,000 g of LDPE was injected into the first layer hopper of the two-layer extruder, 9750 g of LDPE was injected into the second layer hopper, The master batch was changed to 250 g, 750 g, 1250 g, 1750 g, 2500 g, 3750 g and 5000 g in the order of 9250 g, 8750 g, 8250 g, 7500 g, 6250 g and 5000 g in the order of changing the mixing amount of LDPE. And processed into a film.
The thickness of the film thus formed was 40 占 퐉, the thickness of the portion containing carbon nanotubes was 15 占 퐉, and the thickness of the portion where only LDPE was present was 25 占 퐉.
[Experiment 4]
First, a master batch prepared by mixing a conductive silicone polymer and a carbon nanotube at a mixing ratio of 7: 3 by weight was prepared. Then, 10000 g of LDPE was injected into the first layer hopper of the two-layer extruder, 9750 g of LDPE was injected into the second layer hopper, The master batch was changed to 250 g, 750 g, 1250 g, 1750 g, 2500 g, 3750 g and 5000 g in the order of 9250 g, 8750 g, 8250 g, 7500 g, 6250 g and 5000 g in the order of changing the mixing amount of LDPE. And processed into a film.
The thickness of the film thus formed was 40 占 퐉, the thickness of the portion containing carbon nanotubes was 15 占 퐉, and the thickness of the portion where only LDPE was present was 25 占 퐉.
In order to examine the surface conductivities of the films prepared by Experiments 1 to 4, surface resistances were measured at four points on the surface of each film sample, and the average values thereof were shown in Tables 1 to 4 below.
As can be seen from the results of Tables 1 to 4, it was confirmed that as the content of carbon nanotubes increases, the measured value of surface resistance decreases proportionally. Particularly, as shown in Table 3, the conductive silicone polymer and the carbon nanotube When the blend ratio was 6: 4, the measured value of the surface resistance was the smallest. This demonstrates that the carbon nanotube is uniformly impregnated into the base material of the synthetic resin of the carbon nanotube and the conductivity of the carbon nanotube is fully demonstrated.
In addition, it has been confirmed that the master batch in which the carbon nanotubes are mixed using the conductive silicone polymer can be used not only as an additive for the synthetic resin base material used in the film production, but also in the effect that the carbon nanotubes can fully exhibit the conductivity Respectively.
Although the present invention has been described with reference to the preferred embodiments described above, the present invention is not limited thereto but is limited by the claims that follow. Accordingly, those skilled in the art will appreciate that various modifications and changes may be made thereto without departing from the spirit of the following claims.
Claims (14)
Further mixing a conductive liquid silicone polymer containing a metal oxide to a mixture of the carbon nanotubes and the toluene; And
Processing a mixture of the carbon nanotube and the toluene mixed with the conductive liquid silicone polymer containing the metal oxide into a pellet form by using an extruder,
Wherein the mixture of the carbon nanotubes and the toluene is a mixture of 80 to 95 wt% of carbon nanotubes and 5 to 20 wt% of toluene based on the total weight of the mixture
Conductive masterbatch manufacturing method.
The weight ratio of the conductive liquid silicone polymer comprising the carbon nanotubes and the metal oxide to the conductive liquid silicone polymer including the metal oxide may be in the range of 4: 7: 3. ≪ / RTI >
Wherein the conductive liquid silicone polymer has a weight average molecular weight in the range of 1,000 to 800,000 g / mol.
Preparing a synthetic resin base material for film production;
Mixing the synthetic resin matrix and the conductive master batch; And
A step of extruding a synthetic resin base material mixed with the conductive master batch to produce a film
≪ / RTI >
Wherein the synthetic resin base material is one or more of low density polyethylene (LDPE), polyethylene terephthalate (PET), polyvinyl chloride (PVC), and thermoplastic polyurethane (TPU).
In the step of mixing the master batch with the synthetic resin base material,
Wherein the master batch is mixed with 1 to 20 wt%, and the synthetic resin base material is mixed with 80 to 99 wt%.
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| KR102294864B1 (en) | 2017-12-08 | 2021-08-30 | 주식회사 엘지화학 | Conductive silicone composition and silicone composite prepared thereby |
| CN110418821B (en) | 2017-12-08 | 2021-09-10 | Lg化学株式会社 | Polysiloxane composite material and method for producing same |
| CN111564236B (en) * | 2020-04-28 | 2022-11-29 | 清华大学 | Conductive paste, preparation method and preparation method of conductive film |
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| JP2008156478A (en) * | 2006-12-25 | 2008-07-10 | Mitsubishi Rayon Co Ltd | Carbon nanotube-containing composition, production method thereof, and coating film, cured film, composite, resin molding and master batch obtained therefrom, |
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