KR20100080419A - Resin composition - Google Patents
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- KR20100080419A KR20100080419A KR1020090131698A KR20090131698A KR20100080419A KR 20100080419 A KR20100080419 A KR 20100080419A KR 1020090131698 A KR1020090131698 A KR 1020090131698A KR 20090131698 A KR20090131698 A KR 20090131698A KR 20100080419 A KR20100080419 A KR 20100080419A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L81/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen or carbon only; Compositions of polysulfones; Compositions of derivatives of such polymers
- C08L81/04—Polysulfides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/041—Carbon nanotubes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/046—Carbon nanorods, nanowires, nanoplatelets or nanofibres
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L101/00—Compositions of unspecified macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2300/00—Characterised by the use of unspecified polymers
- C08J2300/22—Thermoplastic resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
Abstract
The present invention provides a resin composition comprising (A) a thermoplastic resin, (B) an inorganic material having a volume resistivity of 10 −3 Pa · m or less and a relative permeability of 5,000 or more, and (C) a fiber filler. The resin composition according to the present invention can be used for high stiffness, high electroconductivity, and high performance electromagnetic interference (EMI) and radio frequency interference (RFI) shielding purposes. It can be easily used in a place including the integration, light weight, mass production of electrical / electronic materials and the like.
Description
The present invention relates to a resin composition, and more particularly, to a multifunctional resin composition for shielding high stiffness, high electroconductivity, and high performance electromagnetic interference (EMI) and radio frequency interference (RFI).
With the miniaturization, integration, and lightening of electric / electronic products, moduleization of internal components is becoming an essential item. For example, an internal frame that requires grounding capability must have high mechanical stiffness at the same time as electrical conductivity, and an exterior material that requires EMI / RFI shielding must have excellent appearance characteristics as well as EMI / RFI shielding. In the past, the implementation of the necessary functions was made through a combination of materials having respective characteristics, but the material composite functionality has become an essential item in order to meet the aforementioned requirements for miniaturization, integration, and weight reduction. Including this, high productivity of materials to meet the demands of mass production is also an important item to be considered in advanced materials. The present invention relates to a composite functional material that is easy to mass-produce, and the invention according to the present invention has a high rigidity, high electroconductivity, and EMI / RFI shielding at the same time so that it can be easily used in an electric / electronic product. Resin composition.
As a high stiffness resin composition, high stiffness reinforcing materials such as glass fiber, aramid fiber, and carbon fiber are generally reinforced, so that the characteristics thereof can be realized. In the case of electric conductivity, metals such as copper, aluminum, stainless steel, or graphite, Since carbons such as carbon black and carbon nanotubes are mixed with the polymer, the characteristics thereof can be realized. Well-known techniques are briefly described.
Efficient electromagnetic shielding technology to prevent electromagnetic waves is more and more necessary in modern times, which is due to the high efficiency, high power consumption and highly integrated electrical and electronic products, which can cause other devices and system malfunction or harm the human body. Because.
Conventionally, as a method for shielding electromagnetic waves, there has been a method of using a metal applied with a coating / plating technique. Such metals have a high conductivity (low R value, low impedance) and have a high ratio of electromagnetic shielding through surface reflection of electromagnetic waves, and for this reason, a thin metal can effectively block electromagnetic waves.
However, when the coating / plating technique is described with a plating technique as an example, the process of the plating technique is complicated such as degreasing, etching, neutralization, activation, accelerator, metal deposition, activation, plating primary, secondary plating, tertiary plating, etc. Therefore, in recent years that require high productivity has a disadvantage in terms of production price, productivity and above all environmental.
Conventional technology related to electromagnetic shielding from all electronic devices such as radio frequency interference (RFI) with such electromagnetic shielding is an electromagnetic shielding device including a polymer substrate coated on a metal surface (US Patent Publication No. 20070199738) , An electromagnetic wave shielding material (US Patent Publication No. 20070056769) containing a non-conductive polymer, a conductive polymer and an electrically conductive metal powder, and a conductive fiber were coated with a compatibilizer such as an organic wetting agent, and then composited into a resin to prepare an electrically conductive impregnated fiber. (US Patent Publication No. 20020108699), an electrically conductive thermoplastic elastomer comprising a styrene-ethylene-butadiene-styrene copolymer (SEBS) -based matrix material and a silver-plated nickel conductive matrix, comprising a conductive filler (US Patent No. 20020108699). 6,638,448), carbonaceous blends of two polymer resin blends with different polarities An electrically conductive composition (US Pat. No. 6,409,942) in which a carbonaceous conductive filler is positioned on a highly polarized side by impregnating the conductive filler, and a sheet material or a polymer carrier capable of forming pores during the thermoforming process, and a low melting point metal And thermoformed electromagnetic shielding sheets (US Pat. No. 5,869,412) containing conductive fillers.
They do not offer high stiffness, high conductivity, and EMI / RFI shielding.
An object of the present invention is to provide a composite resin composition of high rigidity, high conductivity, EMI / RFI shielding.
Another object of the present invention is to provide a plastic molded article that can be usefully used in the field of high rigidity, high conductivity and at the same time EMI / RFI shielding is required.
The above and other objects of the present invention can be achieved by the present invention described below.
The present invention provides a resin composition comprising a resin composition composed of (A) a thermoplastic resin, (B) an inorganic material having a volume resistivity of 10 −3 Pa · m or less and a relative permeability of 5,000 or more, and (C) a fiber filler.
The resin composition according to the present invention may further include a carbon-based filler (D).
Preferably, the resin composition comprises (A) 40 to 80% by weight of thermoplastic resin, (B) 3 to 20% by weight of inorganic material having a volume resistivity of 10 −3 Pa · m or less and relative permeability of 5,000 or more, and (C) Fiber filler 5-40% by weight and optionally (D) 0.05-10.0% by weight of the carbon-based filler.
In addition, the present invention provides a plastic molded article comprising the resin composition.
In the composition of the present invention, high stiffness can be achieved through the fiber filler according to the present invention, and consequently, high stiffness, high conductivity, and EMI through inorganic materials having a volume resistivity of 10 -3 3 · m and a relative permeability of 5,000 or more. It is to provide a resin composition having the effect of / RFI shielding properties.
Hereinafter, embodiments of the present invention will be described in detail. However, this is presented as an example, by which the present invention is not limited, and the present invention is defined only by the scope of the following claims.
BACKGROUND OF THE INVENTION Methods for producing high rigidity, high conductivity conductive resin compositions are generally well known. For example, conductive materials such as carbon fibers and carbon nanotubes may be combined with resin alone or in combination with other reinforcing materials. Its method is well known and will be briefly described. However, in the case of using carbonaceous conductive materials, there is a limit of EMI / RFI shielding, and thus, another additional method is required to obtain specially reinforced EMI / RFI characteristics. The present invention provides a resin composition having high stiffness, high electroconductivity, and EMI / RFI shielding properties.
In the following Equation 1 representing the electromagnetic wave shielding efficiency, the electromagnetic shielding effectiveness (S.B.) could be improved by not only improving the electromagnetic wave reflection but also improving the internal absorption rate.
[Equation 1]
S.B. = R + A + B
Where R is the surface reflection of the electromagnetic wave (electrical conductivity), A is the internal absorption of the electromagnetic wave, and B is the loss through multiple reflections.
In the case of the resin composition, since the electrical conductivity is lower than that of the metal, it is important to improve not only surface reflection but also internal absorption among the items shown in the above formula (1). Therefore, in order to increase the electromagnetic shielding efficiency of the resin composition, it is necessary to increase the value of A, that is, increase the value of A based on lowering the surface impedance (by increasing the electrical conductivity) to increase the R value. Compound resin can be made.
That is, the present inventors have found that the electromagnetic wave shielding efficiency of the resin composition should increase the internal absorption of the electromagnetic wave as well as the electromagnetic shielding through the improvement of the electrical conductivity. The internal absorption of the electromagnetic wave is directly related to the permeability of the material. Because of this, a material having a high permeability can be introduced. It is important to note that non-conductive materials such as materials that have high permeability, such as Sendust or Ferrite, have little effect on EMI / RFI shielding of the resin composition, but are electrically conductive and high permeability inorganic materials such as mumetal (Mu). -metal) or permalloy is very effective for EMI / RFI shielding of resin compositions. These inorganic materials are not only effective in absorbing electromagnetic waves due to their high permeability, but also have good electrical conductivity, which together with the carbon fibers and carbon nanotubes used, help to form an electrically conductive pass in the resin composition, thereby improving electrical conductivity.
The electromagnetic wave shielding material using the resin composition is a very economical method in terms of production price and productivity since it can be commercialized only by injecting a composite resin.
The resin composition for high stiffness, high conductivity, and EMI / RFI shielding of the present invention includes (A) a thermoplastic resin, (B) an inorganic material having a volume resistivity of 10 −3 Ω · m or less and a relative permeability of 5,000 or more, and (C) a fiber filler. It includes.
The fiber filler of the above (C) is preferably at least one selected from carbon fiber, glass fiber, boron fiber, synthetic amide fiber and liquid crystalline polyester fiber.
Preferably, the resin composition according to the present invention may further include (D) a carbon-based filler, the (D) carbon-based filler, for example, a group consisting of carbon nanotubes, carbon black and carbon nanofibers At least one selected from.
In the resin composition of the present invention, the content of the thermoplastic resin is 40 to 80% by weight, the electrically conductive and high permeability inorganic material is 3 to 20% by weight, the content of the fiber filler is 5 to 40% by weight, and the carbon-based filler Content is It is a composite resin composition for high stiffness, high conductivity, and electromagnetic interference / radio frequency interference shielding, which is 0.05 to 10.0% by weight and the sum of all components is 100% by weight.
The resin composition of the present invention having the above constitution is manufactured by a process step of mixing the components, and has a structure in which the thermoplastic resin forms a matrix and the fillers are dispersed in the matrix.
Hereinafter, each component of the present invention will be described in detail.
(A) thermoplastic resin
Specific examples of the thermoplastic resin of the present invention include polyamide; Polyalkylene terephthalates such as polyethylene terephthalate or polybutylene terephthalate; Polyacetals; Polycarbonate; Polyimide; Polyphenylene oxide; Polysulfones; Polyphenylene sulfide; Polyamide imide; Polyether sulfones; Liquid crystal polymer; Polyether ketones; Polyetherimide; Polyolefins such as polypropylene or polyethylene; Acrylonitrile butadiene styrene; polystyrene; Syndiotactic polystyrene; Etc. can be mentioned. It is also possible to use those selected from the group consisting of these blends and combinations thereof.
Preferably, the thermoplastic resin (A) of the present invention is a crystalline thermoplastic resin. Such a crystalline thermoplastic resin has the advantage of forming a conductive pass better than an amorphous resin due to its property of rejecting fillers (other components other than the component (A) in the resin composition of the present invention) out of the crystal region during its crystallization. have. In addition, in terms of mechanical rigidity, the reinforcing effect of the filler is much better than that of the amorphous resin.
The crystalline thermoplastic resin is preferably a group consisting of polyamide, polyethylene terephthalate, polybutylene terephthalate, polyacetal, polyphenylene sulfide, liquid crystal polymer, polyetherketone, polyolefin, syndiotactic polystyrene, and mixtures thereof. Can be selected from.
The content of the thermoplastic resin in the resin composition of the present invention is preferably 40 to 80% by weight, more preferably 60 to 75% by weight. When the content of the thermoplastic resin is 40% by weight or less, it is difficult to process the resin composition, and when the content of the thermoplastic resin is 80% by weight or more, it is difficult to implement the target physical properties of the present invention.
(B) electrically conductive and high permeability minerals
The electrically conductive, high permeability inorganic material of the present invention can preferably be used an inorganic material selected from the group classified into inorganic materials having a volume resistivity of 10 −3 [Ω · m] or less and a relative permeability of 5,000 or more. In more detail, Mu-metal or Permalloy which are nickel-iron alloys can be used preferably.
In the resin composition of the present invention, an electrically conductive and high permeability inorganic material may be preferably used in an amount of 3 to 20% by weight, and more preferably 5 to 15% by weight. When the content of the inorganic material is less than 3% by weight, the EMI / RFI shielding property is inadequately low. If the content is more than 20% by weight, the viscosity and specific gravity of the resin composition are adversely affected.
(C) fiber filler
The (C) fiber filler of the present invention is preferably at least one selected from carbon fiber, glass fiber, boron fiber, synthetic amide fiber and liquid crystalline polyester fiber.
The carbon fibers may be preferably selected from the group classified into conventional carbon fibers of the PAN series or the Pitch series. More specifically, an average diameter of 5 ~ 12μm, an average length of 3 ~ 12mm, the volume resistivity 10-3 can be preferably used an [Ω and m] or less carbon fiber tensile stiffness than 100GPa.
The glass fiber can be used for the purpose of improving the strength while at the same time canceling the fracture characteristics of the resin composition generated when using only carbon fiber can be used conventional glass fiber, preferably, reinforcing physical properties High rigid glass fibers used for the purpose of doing so can be used. In one embodiment, glass fibers having an average diameter of 8 to 15 µm and an average length of 2 to 12 mm can be preferably used.
The fiber filler of the present invention is mainly responsible for the electrical conductivity and high stiffness of the resin composition, the lower the volume resistance, the higher the tensile stiffness can be used more preferably.
In the resin composition of the present invention, the fiber filler is preferably 5 to 40% by weight, more preferably 10 to 25% by weight. When the content of the fiber filler is 5% by weight or less, it is difficult to realize the target physical properties of the present invention. When the content of the fiber filler is 40% by weight or more, the workability is inferior, and a molded article made from such a resin composition is brittle even in a small impact.
(D) Carbon Filler
In the resin composition of the present invention, one or more selected from the group consisting of carbon nanotubes, carbon black and carbon nanofibers may be used as the carbon-based filler (D). Preferably, carbon nanotubes are used, because among them, electrostatic discharge (ESD) of carbon nanotubes exhibits the best performance.
The carbon nanotubes are divided into single wall carbon nanotubes, double wall carbon nanotubes, and multiwall carbon nanotubes according to the number of walls thereof. It can be selected from and used as a mixture thereof. More specifically, carbon nanotubes having an average outer diameter of 1 to 50 nm, an average length of 10 nm to 20 µm, and a purity of 80% or more can be preferably used.
In the resin composition of the present invention, the content of the (D) carbon-based filler is preferably 0.05 to 10.0% by weight, more preferably 0.3 to 5.0% by weight. When the content of the carbon-based filler (D) is 0.05% by weight or less, it is difficult to implement the target physical properties of the present invention. When the content of the carbon-based filler is 10.0% by weight or more, the viscosity of the resin composition is rapidly increased, and thus the process for the resin composition is difficult.
Another aspect of the present invention provides a molded article produced using the resin composition according to the present invention. The molded article of the present invention can be usefully used in the field of high rigidity, high conductivity and at the same time EMI / RFI shielding is required. In particular, it can be usefully applied to the production of various molded products, such as display devices such as TV, PDP, components of electrical and electronic products such as computers, mobile phones and office automation equipment, internal frames.
In one embodiment, the plastic molded article according to the present invention has an electromagnetic shielding value of 15 to 50 dB, the surface resistance measured according to ASTM D257 is 10 ~ 10 4 Ω / □, ASTM at 1/4 "thickness The flexural strength measured according to D790 is 12-30 GPa and the notched Izod impact strength measured according to ASTM D256 at 1/8 "thickness may be 25-70 J / m.
The present invention will be further illustrated by the following examples, which are merely illustrative of the present invention and are not intended to limit or limit the scope of the present invention. Details that are not described herein will be omitted since those skilled in the art can sufficiently infer technically.
Example
Hereinafter, the configuration and operation of the present invention through the preferred embodiment of the present invention will be described in more detail. However, this is presented as a preferred example of the present invention and in no sense can be construed as limiting the present invention.
(A) thermoplastic resin
As the thermoplastic resin used in the present invention, a polyphenylene sulfide (PPS) resin having a melt index (MFI) having a value of 48 to 70 g / 10 min at a load of 316 ° C. and 1270 g was used.
(B) electrically conductive and high permeability minerals
The electrically conductive and high permeability inorganic material used in the present invention is a nickel-iron alloy Permalloy (Dongbu Precision Chemical Co., Ltd.), whose volume resistivity is 10 -7 [μm] and the relative permeability is 10,000.
(C1) fiber filler
As the carbon fiber used as the fiber filler in the present invention, a pitch-based carbon fiber having a diameter of 7 μm, a length of 4 mm, a volume resistivity of 10 −5 [μm · m], and a tensile strength of 200 GPa was used.
(C2) fiber filler
Glass fiber used as the fiber filler in the present invention is a glass fiber 10μm in diameter, 3mm in length and the surface coating as a Silane-based compatibilizer to improve the interfacial adhesion with PPS used as the thermoplastic resin
(D) Carbon Filler
The carbon nanotubes used as the carbon-based filler used in the present invention used a multi-walled carbon nanotube having a diameter of 9.5 nm, a length of 1.5 μm, and a purity of 90%.
After preparing the resin composition by mixing the above-mentioned components in the compositions shown in Examples 1 to 6 and Comparative Example 1 of Table 1, using a conventional twin screw extruder and injection machine for the measurement of physical properties Specimen was prepared.
The surface resistance of the prepared specimens was measured according to ASTM D257.
Flexural strength was measured according to ASTM D790 specification at 1/4 "thickness.
Notched Izods were measured according to ASTM D256 specification at 1/8 "thickness.
EMI shielding rate was measured by a spectrum analyzer manufactured by ROHDE & SCHWARZ.
The physical property measurement results are shown in Table 1 below.
Carbon fiber (C1) used as a fiber filler from the resin composition of the Examples and Comparative Examples of Table 1 mainly contributes to the rigidity and electrical conductivity, carbon-based fillers are indispensable contribution to the electrical conductivity, as a fiber filler The glass fiber (C12) used contributes to the reinforcement of the physical properties, but especially to the impact strength. In particular, permalloy used as an electrically conductive and high permeability inorganic material (B) is used to improve carbon fiber and carbon nanotubes. It can be seen that the limiting EMI / RFI shielding characteristics are greatly improved.
This can be more clearly understood through the fact that EMI / RFI shielding properties are deteriorated when the firmware is removed in the comparative example.
In conclusion, the present invention provides a multifunctional resin composition having high stiffness, high conductivity, and EMI / RFI shielding properties through an optimized mixing of electrically conductive, high permeability inorganic material, fiber filler, and optionally carbon-based filler.
The present invention is not limited to the above embodiments, but may be manufactured in various forms, and a person skilled in the art to which the present invention pertains has another specific form without changing the technical spirit or essential features of the present invention. It will be appreciated that the present invention may be practiced as. It is therefore to be understood that the above-described embodiments are illustrative in all aspects and not restrictive.
Claims (18)
Priority Applications (2)
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US12/648,368 US7939167B2 (en) | 2008-12-30 | 2009-12-29 | Resin composition |
EP20090180952 EP2204403A1 (en) | 2008-12-30 | 2009-12-30 | Resin composition |
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KR20080136316 | 2008-12-30 | ||
KR1020080136316 | 2008-12-30 |
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JP5173143B2 (en) * | 2006-03-28 | 2013-03-27 | パナソニック株式会社 | Electromagnetic wave shielding resin composition and molded product thereof |
JP2007261100A (en) * | 2006-03-28 | 2007-10-11 | Matsushita Electric Works Ltd | Electromagnetic wave shield molded product, its manufacturing method, and resin mold material |
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US7999018B2 (en) * | 2007-04-24 | 2011-08-16 | E. I. Du Pont De Nemours And Company | Thermoplastic resin composition having electromagnetic interference shielding properties |
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2009
- 2009-12-28 JP JP2009297919A patent/JP2010155993A/en active Pending
- 2009-12-28 KR KR1020090131698A patent/KR101267272B1/en not_active IP Right Cessation
- 2009-12-30 CN CN2009102589274A patent/CN101768367B/en not_active Expired - Fee Related
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Cited By (4)
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KR101397687B1 (en) * | 2010-08-20 | 2014-05-23 | 제일모직주식회사 | High modulus composite for emi shielding |
WO2014163255A1 (en) * | 2013-04-01 | 2014-10-09 | 제일모직주식회사 | Thermoplastic resin composition and moulded article having outstanding antistatic properties |
KR20150066480A (en) * | 2013-12-06 | 2015-06-16 | 주식회사 엘지화학 | Thermoplastic resin composition for radar cover |
US9840609B2 (en) | 2013-12-06 | 2017-12-12 | Lg Chem, Ltd. | Thermoplastic resin composition for radar cover |
Also Published As
Publication number | Publication date |
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TW201024352A (en) | 2010-07-01 |
CN101768367B (en) | 2012-07-04 |
TWI404758B (en) | 2013-08-11 |
KR101267272B1 (en) | 2013-05-23 |
JP2010155993A (en) | 2010-07-15 |
CN101768367A (en) | 2010-07-07 |
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