KR20140132961A - Thermally conductive polymer compositions based on hybrid system, methods for preparing the same and shaped articles using the same - Google Patents
Thermally conductive polymer compositions based on hybrid system, methods for preparing the same and shaped articles using the same Download PDFInfo
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- KR20140132961A KR20140132961A KR1020130052357A KR20130052357A KR20140132961A KR 20140132961 A KR20140132961 A KR 20140132961A KR 1020130052357 A KR1020130052357 A KR 1020130052357A KR 20130052357 A KR20130052357 A KR 20130052357A KR 20140132961 A KR20140132961 A KR 20140132961A
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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
- C08K3/041—Carbon nanotubes
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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
- C08L101/12—Compositions of unspecified macromolecular compounds characterised by physical features, e.g. anisotropy, viscosity or electrical conductivity
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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
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
Abstract
The present invention relates to a polymer composition comprising a thermally conductive filler and a single-walled carbon nanotube mixed at a predetermined ratio, and a method for producing the same.
When the thermally conductive filler having a plate-like shape is mixed with the single-walled carbon nanotubes to improve the contact ratio between the fillers, the polymeric composition prepared in the present invention can be used as a single- There is an excellent effect that the thermal conductivity is improved more than when the tube is used. In addition, since a filler commercialized as a thermally conductive filler is used and the manufacturing process is simple, the manufacturing cost is low and mass production can be performed, and thus it can be widely used in the electronic parts industry and the semiconductor industry.
Description
The present invention relates to a thermally conductive polymer composition using a hybrid filler system and a method for producing the same.
2. Description of the Related Art As electronic devices such as smart phones and computers have become smaller and lighter, there has been a demand for high-density packaging of semiconductor packages and high integration and speeding up of devices in integrated circuits. Accordingly, heat generated from various electronic components is discharged to the outside to prevent damage to the component due to heat, so that research on a heat radiating plate or a heat radiating sheet has been actively conducted.
As a conventional heat sink, a heat-dissipating plate such as aluminum, for example, of a metal having good thermal conductivity is used. However, when metal is used as a heat sink material, there are limitations on low formability, productivity and part design, and research is being conducted to replace this material.
In addition, the heat-radiating sheet is attached to a part or product that generates heat such as a light-emitting diode (LED) or a battery and a printed circuit board (PCB), and has a high heat radiation effect. Currently, a thermally conductive polymer have.
The thermally conductive polymer is prepared by adding a thermally conductive filler having a high thermal conductivity to a polymer which is a heat resistor. In addition, the development of the thermally conductive polymer material has been proceeded in order to obtain an optimal thermal conductivity with a minimum thermally conductive filler content in order to enable injection molding and ensure appropriate physical properties.
The following techniques are known as a conventional method for producing a thermally conductive polymer.
Patent Document 1 relates to a polyamide resin composition excellent in whiteness degree, thermal conductivity and extrusion moldability, and a method for producing the same. The polyamide resin is compatible with a thermally conductive filler, a filler and a polyamide and has a weight average molecular weight of 500,000 - And a method for producing a polyamide resin composition excellent in whiteness, thermal conductivity and extrusion moldability, which comprises thermoplastic resin having a molecular weight of 5,000,000 to 5,000,000.
The present invention can simultaneously obtain high whiteness and thermal conductivity by using boron nitride as the thermally conductive filler. However, in order to compensate the mechanical strength and moldability of the thermally conductive polymer to be produced, a separate filler, a white pigment, Use a polymer resin that is compatible with the polyamide resin used.
Patent Document 2 discloses a resin composition having excellent heat resistance, reflectance and thermal conductivity, and a method for producing the resin composition. The resin composition comprises 40 to 70 wt% of a crystalline resin having a melting point of 270 캜 or higher, 5 to 50 wt% To 40% by weight and a stiffness increase of 5% to 30% by weight in a twin-screw extruder having a barrel temperature of 280 to 360 ° C to produce a pellet-shaped material will be. The average thermal conductivity of the polymer composition prepared according to the present invention is 0.5 W / m · K, and a stiffness-increasing agent is further used to compensate for mechanical properties.
Further, D. Khastgir et al. Conducted experiments on the effect of carbon-based fillers having different shapes and sizes on properties related to electrical conductivity and the like of ethylene-vinyl acetate copolymer (Non-Patent Document 1).
In the above experiment, graphite was used as an electrically conductive filler, and short carbon fibers and multiwall carbon nanotubes were used. As a result of the experiments, short carbon fibers and multiwall carbon nanotubes having a larger aspect ratio than graphite, which is an electrically conductive filler, The polymer composition thus obtained showed a high electrical conductivity by percolation at a low content (Non-Patent Document 1).
However, since the multi-walled carbon nanotube does not have a high thermal conductivity, a high-content multi-walled carbon nanotube should be included in order to obtain a thermally conductive polymer composition having desired properties. As a result, the mechanical properties are deteriorated, And it is difficult to commercialize it.
Thus, the present inventors have succeeded in producing a polymer composition having improved thermal conductivity by improving the contact ratio between thermally conductive fillers by using a hybrid filler system comprising a mixture of a plate-shaped thermally conductive filler and a small amount of single wall carbon nanotubes in a polymer resin And completed the present invention.
1. Patent Document 1: Korean Patent Publication No. 10-2011-0079146
2. Patent Document 2: Korean Patent Laid-Open No. 10-2009-0088134
3. Non-Patent Document 1: NJS Sohi Sambhu Bhadra and D. Khastgir, Carbon volume 49,
An object of the present invention is to provide a thermally conductive polymer composition using a hybrid filler system and a method for producing the same.
It is still another object of the present invention to provide a molded article using the polymer composition and a method for producing the same.
In order to achieve the above object, the present invention provides a thermally conductive polymer composition comprising a heat-resistant polymer resin, a thermally conductive filler, and a non-surface treated single-walled carbon nanotube.
The present invention also provides a method for producing the thermally conductive polymer composition, comprising melting and mixing a heat-resistant polymer resin, a carbon-based plate-shaped thermally conductive filler, and a non-surface-treated carbon nanotube in a melt mixing apparatus.
The present invention also provides a molded article comprising the thermally conductive polymer composition and a method for producing the same.
The thermally conductive polymer composition produced by the present invention has an effect of improving the thermal conductivity by improving the contact ratio by forming an effective network between the plate-shaped thermally conductive fillers by using the plate-shaped thermally conductive filler and the single wall carbon nanotube. In addition, since a commercialized filler is used and a manufacturing process is simple, it can be widely used in an electronic parts industry, a semiconductor industry, and the like.
1 is a schematic view showing an enlarged view of a polymer composition containing only a conventional thermally conductive filler,
FIG. 2 is an enlarged schematic view of a polymer composition using mixed thermally conductive polymer fillers and surface-treated single-walled carbon nanotubes according to an embodiment of the present invention, and FIG.
FIG. 3 is an enlarged view of a polymer composition in which thermally conductive polymer fillers according to an embodiment of the present invention are mixed with non-surface-treated single-walled carbon nanotubes.
Hereinafter, the present invention will be described in detail.
According to the present invention,
5 to 90% by weight of a heat resistant polymer resin;
5 to 90% by weight of thermally conductive filler; And
1 to 5 wt% non-surface treated single walled carbon nanotubes;
And a thermally conductive polymer composition.
In the composition according to the present invention, the heat-resistant polymer resin may be a polyamide (PA), a liquid crystal polymer (LCP), a polyphenylene sulfide (PPS), a polycarbonate (PC) Polymeric materials capable of maintaining physical properties including mechanical and electrical properties are usable, and their use is not particularly limited. As a suitable example of the heat-resistant polymer resin used in the present invention, polyamide (PA) is excellent in heat resistance, rigidity and stability, and the polymer composition containing the polyamide can be used for electronic parts and precision molded parts.
At this time, the content of the heat-resistant polymer resin is preferably 5 to 90% by weight, more preferably 35 to 85% by weight. In the case of a thermally conductive polymer composition containing less than 5% by weight of the heat resistant resin, mechanical properties and moldability are lowered and productivity and component design are limited. When the content of the heat resistant resin exceeds 90% by weight, It is difficult to obtain the thermally conductive polymer composition of the present invention.
In the composition according to the present invention, the thermally conductive filler can be used without limitation as long as it can improve the contact ratio between pillars, but it is preferable to use a plate-like filler or a fibrous filler. More preferably, And graphite nanoparticles can be used more preferably.
Specifically, assuming that externally supplied heat travels in the polymer, the heat-resistant polymer does not have a medium capable of transferring heat, and most of the heat transferred in the polymer is lost. However, when the polymer includes a thermally conductive filler, the filler becomes a medium for transferring heat, and heat can be transferred to the outside. Therefore, heat supplied from the outside can be discharged to the outside more effectively as the contact ratio between the thermally conductive fillers increases.
In the present invention, by using a mixture of the plate-shaped thermally conductive filler and the carbon nanotube, the thermal conductivity of the polymer composition prepared by improving the contact ratio of the filler by filling the carbon nanotubes between the plate-shaped thermally conductive fillers in the polymer can be improved .
The contact area of the thermally conductive filler included in the polymer composition according to the present invention varies depending on the shape. It is advantageous to improve the thermal conductivity of a polymer composition by using a sheet or plate-like filler which makes contact with a line or a surface rather than a spherical or tube-shaped filler which makes point contact. Based ceramic filler may be used.
The thermally conductive filler is preferably 5 to 90% by weight, more preferably 10 to 60% by weight. When the content of the thermally conductive filler is less than 5% by weight, there is a problem in that it is difficult to obtain thermal conductivity, which is a desired property of the polymer composition to be produced. When the content of the thermally conductive filler is more than 90% by weight, There is a problem that the viscosity is too high and the moldability is deteriorated.
The present invention also provides a method for producing the thermally conductive polymer composition, comprising melting and mixing a heat-resistant polymer resin, a carbon-based plate-shaped thermally conductive filler, and a non-surface-treated carbon nanotube in a melt mixing apparatus.
Specifically, the manufacturing method includes a step of melt-mixing a carbon-based plate-shaped thermally conductive filler and a non-surface-treated single-walled carbon nanotube in a heat-resistant polymer resin in a melt-mixing apparatus. Through the above steps, the heat resistant polymer resin, the thermally conductive filler, and the non-surface treated single-walled carbon nanotube are uniformly mixed.
In the production method according to the present invention, the melt mixing apparatus may use a twin-screw extruder. The melting and mixing of the heat-resistant polymer resin with the plate-shaped thermally conductive filler and the single-walled carbon nanotube can be performed by a known method using a device such as a twin-screw extruder. On the other hand, the mixing of the heat-resistant polymer resin with the thermally conductive filler and the non-surface treated single-walled carbon nanotubes proceeds by the melting process, and since the solvent is not used at all, it is an environmentally friendly process and can simplify the process .
In the production method according to the present invention, it is preferable that the melt mixing is performed at a temperature of 250 to 350 ° C. When the heat-resistant polymer resin, the thermally conductive filler, and the non-surface treated single-walled carbon nanotube are melted and mixed at a temperature lower than 250 ° C, the heat-resistant polymer resin and the thermally conductive filler and the carbon nanotube are not uniformly mixed. When the temperature exceeds 350 ° C, there is a problem that the physical properties of the heat-resistant polymer resin are lowered due to thermal decomposition.
On the other hand, the mixing of the heat-resistant polymer resin with the thermally conductive filler and the non-surface-treated carbon nanotube can appropriately select the melt-mixing temperature according to the heat-resistant polymer resin and the thermally conductive filler to be used.
The present invention also provides a molded polymer article comprising the thermally conductive polymer composition.
The present invention also provides a method for producing the polymer molded article by injection molding the thermally conductive polymer composition.
The polymer composition prepared by the method of the present invention is excellent in thermal conductivity and can be applied to parts for emitting heat generated in electronic equipment.
Hereinafter, embodiments of the present invention will be described in more detail. However, the following examples are illustrative of the present invention, and the contents of the present invention are not limited by the following examples.
< Example 1> Preparation of Thermally Conductive Polymer Composition 1
, 84.15% by weight of polyamide (PA 300, KP chemtech, EN 300) as thermostable polymer resin, 14.85% by weight of graphite nanopletelet (GNP (Graphite nanopletelet), Timcal) as thermally conductive filler, (DSM Xplore, DSM Xplore micro-compounder) to prepare pellets of the polymer composition. The pellets were prepared by mixing 1 wt% of a polyolefin (SWNT, Single Walled Carbon Nanotube) At this time, the extrusion temperature was 280 占 폚.
< Example 2-6> Preparation of Thermally Conductive Polymer Composition 2
(PA, KP chemtech, EN 300) as the heat-resistant polymer resin in the mixed solution of Example 1, the weight percentage of graphite nanoplet (GNP (Graphite nanopletelet), Timcal) as thermally conductive filler, Pellets of a polymer composition were prepared in the same manner as in Example 1, except that the weight percentages of single walled carbon nanotubes (SWNTs, Nanocyl) were mixed as shown in Table 1 below.
< Example 7> Production of molded article using thermally conductive polymer composition 1
The pellets of the polymer composition prepared in Example 1 were injection-molded by an injection molding machine (DSM Xplore, DSM Xplore micro-injection molding machine) to prepare a molded article of a polymer composition having thermal conductivity and heat resistance.
≪ Comparative Example 1-9 &
(PA, KP chemtech, EN 300) as the heat-resistant polymer resin in the mixed solution of Example 1, the weight percentage of graphite nanoplet (GNP (Graphite nanopletelet), Timcal) as thermally conductive filler, Except that the weight% of the surface-treated single-walled carbon nanotubes (SWNT [-COOH] (Functionalized single walled carbon nanotube), Nanocyl) was mixed as shown in Table 1 below. Of pellets were prepared.
"*" Indicates surface treated carbon nanotubes (SWNT [-COOH])
< Experimental Example 1> Measurement of Thermal Conductivity of Polymer Composition
The following experiments were conducted to measure the thermal conductivity of the polymer compositions prepared in Examples 1 to 6 and Comparative Examples 1 to 9 of the present invention. The thermally conductive polymer compositions prepared according to Examples 1 to 6 and Comparative Examples 1 to 9 of the present invention were measured for thermal diffusivity according to ASTM E1461 at a temperature of 25 캜 using a Netzsch LFA 447 measuring instrument (Netzsch) Specific heat was measured according to ASTM E1952 using an MDSC measuring instrument (TA instrument), and the density was measured according to ASTM D6226 using a gas pycnometer (Protech). Then, thermal conductivity (κ) was calculated by substituting the thermal diffusivity, specific heat and density obtained by the above experiment according to the following Equation 1, and the results are shown in Table 2 below.
[Equation 1]
Thermal conductivity (κ) = thermal diffusivity (α) X Specific heat (Cp) X density (ρ)
Table 2 shows that the amount of the plate-shaped thermally conductive filler in the polyamide (PA) is 5 to 90% by weight based on the total weight of the thermally conductive polymer composition, the plate-like thermally conductive filler (GNP) The thermal conductivity of a polymer composition prepared by mixing a nanotube (SWNT) or a surface-treated single-walled carbon nanotube (SWNT [-COOH]) with the plate-shaped thermally conductive filler (GNP) .
According to Table 2, the thermal conductivity of the thermally conductive polymer composition prepared by using the plate-shaped thermally conductive filler showed a higher thermal conductivity as the weight percentage of the plate-shaped thermally conductive filler was larger, and the carboxylated surface-treated single walled carbon nanotube (SWNT [ - COOH]), the thermal conductivity was higher when single wall carbon nanotubes (SWNTs) without surface treatment were mixed together.
Specifically, Example 1 and Comparative Example 1; Example 2 and Comparative Example 2; Examples 1 and 2 and 3 show the results of the comparison of Example 3 and Comparative Example 3 in that the compositions of the comparative two thermally conductive polymer compositions were similar to those of the non-surface treated single wall carbon tubes (SWNTs ), The values of the thermal conductivity values were increased by about 0.469 W / mK, 1.293 W / mK, and 1.827 W / mK, respectively in the above-described order.
As a result, it was found that the thermal conductivity was improved when the single-walled carbon nanotubes were mixed with the single-walled carbon nanotubes rather than using the single-walled thermally conductive filler alone. The rate of increase is increased.
In order to solve the problem of dispersion, surface-treated single-walled carbon nanotubes (SWNT [-COOH]) were used for surface-treated single-walled carbon nanotubes (SWNT [-COOH] The surface interaction is good and the contact with the thermally conductive filler becomes less than in the case of the single-walled carbon nanotube which is not surface-treated. In the case of using the single-walled carbon nanotube not subjected to the surface treatment, (SWNT [-COOH]) was used.
Specifically, Example 1 and Comparative Example 4, Example 2 and Comparative Example 5, Example 3 and Comparative Example 6, Example 4 and Comparative Example 7, Example 5 and Comparative Example 8, Example 6 and Comparative Example 9 The composition ratios of the polyamide, the thermally conductive filler and the single-walled carbon nanotube of each thermally conductive polymer composition were the same, but Examples 1 to 6 were different from those of Comparative Examples 4 to 9, The thermal conductivity values of the Examples were 0.121 W / m · K, 0.168 W / m · K, 0.590 W / m · K, and 0.153 W / m 2 · K, 0.588 W / m · K, and 1.089 W / m · K, respectively.
Claims (10)
5 to 90% by weight of thermally conductive filler; And
1 to 5 wt% non-surface treated single walled carbon nanotubes;
And a thermally conductive polymer composition.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10256188B2 (en) | 2016-11-26 | 2019-04-09 | Texas Instruments Incorporated | Interconnect via with grown graphitic material |
| US10529641B2 (en) | 2016-11-26 | 2020-01-07 | Texas Instruments Incorporated | Integrated circuit nanoparticle thermal routing structure over interconnect region |
| US10811334B2 (en) | 2016-11-26 | 2020-10-20 | Texas Instruments Incorporated | Integrated circuit nanoparticle thermal routing structure in interconnect region |
| US10861763B2 (en) | 2016-11-26 | 2020-12-08 | Texas Instruments Incorporated | Thermal routing trench by additive processing |
| US11004680B2 (en) | 2016-11-26 | 2021-05-11 | Texas Instruments Incorporated | Semiconductor device package thermal conduit |
| WO2021107722A1 (en) * | 2019-11-29 | 2021-06-03 | 롯데케미칼 주식회사 | Polyolefin-based resin foam, and molded product produced therefrom |
| CN114989608A (en) * | 2022-07-01 | 2022-09-02 | 宁夏清研高分子新材料有限公司 | Heat-conducting polysulfone composite material and preparation method thereof |
| US11676880B2 (en) | 2016-11-26 | 2023-06-13 | Texas Instruments Incorporated | High thermal conductivity vias by additive processing |
| CN114746492B (en) * | 2019-11-29 | 2024-04-19 | 乐天化学株式会社 | Polyolefin resin foam and molded product produced therefrom |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10256188B2 (en) | 2016-11-26 | 2019-04-09 | Texas Instruments Incorporated | Interconnect via with grown graphitic material |
| US10529641B2 (en) | 2016-11-26 | 2020-01-07 | Texas Instruments Incorporated | Integrated circuit nanoparticle thermal routing structure over interconnect region |
| US10790228B2 (en) | 2016-11-26 | 2020-09-29 | Texas Instruments Incorporated | Interconnect via with grown graphitic material |
| US10811334B2 (en) | 2016-11-26 | 2020-10-20 | Texas Instruments Incorporated | Integrated circuit nanoparticle thermal routing structure in interconnect region |
| US10861763B2 (en) | 2016-11-26 | 2020-12-08 | Texas Instruments Incorporated | Thermal routing trench by additive processing |
| US11004680B2 (en) | 2016-11-26 | 2021-05-11 | Texas Instruments Incorporated | Semiconductor device package thermal conduit |
| US11676880B2 (en) | 2016-11-26 | 2023-06-13 | Texas Instruments Incorporated | High thermal conductivity vias by additive processing |
| WO2021107722A1 (en) * | 2019-11-29 | 2021-06-03 | 롯데케미칼 주식회사 | Polyolefin-based resin foam, and molded product produced therefrom |
| CN114746492A (en) * | 2019-11-29 | 2022-07-12 | 乐天化学株式会社 | Polyolefin-based resin foam and molded product produced therefrom |
| CN114746492B (en) * | 2019-11-29 | 2024-04-19 | 乐天化学株式会社 | Polyolefin resin foam and molded product produced therefrom |
| CN114989608A (en) * | 2022-07-01 | 2022-09-02 | 宁夏清研高分子新材料有限公司 | Heat-conducting polysulfone composite material and preparation method thereof |
| CN114989608B (en) * | 2022-07-01 | 2024-01-30 | 宁夏清研高分子新材料有限公司 | Heat-conducting polysulfone composite material and preparation method thereof |
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