WO2018093030A1 - Silicone composition having excellent heat dissipation properties - Google Patents

Silicone composition having excellent heat dissipation properties Download PDF

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Publication number
WO2018093030A1
WO2018093030A1 PCT/KR2017/010010 KR2017010010W WO2018093030A1 WO 2018093030 A1 WO2018093030 A1 WO 2018093030A1 KR 2017010010 W KR2017010010 W KR 2017010010W WO 2018093030 A1 WO2018093030 A1 WO 2018093030A1
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Prior art keywords
silicone composition
silicone
composition
heat dissipation
particle size
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PCT/KR2017/010010
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French (fr)
Korean (ko)
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유일혁
이장민
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주식회사 케이씨씨
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Priority to MYPI2019002002A priority Critical patent/MY192453A/en
Priority to CN201780068534.XA priority patent/CN109906249A/en
Publication of WO2018093030A1 publication Critical patent/WO2018093030A1/en

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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
    • C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04—Polysiloxanes
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • 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
    • C08K3/28—Nitrogen-containing compounds
    • 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
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2296—Oxides; Hydroxides of metals of zinc
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/001—Conductive additives
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/005—Additives being defined by their particle size in general

Definitions

  • the present invention relates to silicone compositions used to improve the heat dissipation of electronic products.
  • a heat dissipating composition in which a filler such as zinc oxide powder or aluminum oxide powder is blended with silicone oil is known.
  • compositions in which other fillers are added to the silicone oil together with zinc oxide powder and aluminum oxide powder, or fillers such as diamond, boron nitride and carbon nanotubes having high thermal conductivity are also known.
  • the thermally conductive material may improve heat dissipation of electronic products by including various fillers, but due to the high content of fillers, the fluidity and handleability of the thermally conductive material may be deteriorated, and thus many practical applications are applied to electronic products. I'm having a hard time.
  • the present invention is to provide a silicone composition having excellent heat dissipation and excellent fluidity, handleability and the like.
  • the present invention comprises a filler comprising a silicon macromer having a content of an alkoxy group bonded to a silicon atom of 0.1 to 1 mol%, silica, and at least two selected from the group consisting of zinc oxide, aluminum oxide and aluminum nitride.
  • a silicone composition comprising a silicon macromer having a content of an alkoxy group bonded to a silicon atom of 0.1 to 1 mol%, silica, and at least two selected from the group consisting of zinc oxide, aluminum oxide and aluminum nitride.
  • the silicone macromer may have a viscosity of 10 to 50 mPa ⁇ s at 25 ° C.
  • the silicone macromer may be a compound represented by Formula 1 below.
  • n is an integer of 8 to 48.
  • the mixing ratio (a: b: c) of the zinc oxide (a), the aluminum oxide (b) and the aluminum nitride (c) may be a weight ratio of 1: 1.20 to 1.45: 0 to 0.6.
  • the average particle size (D 50 ) of the zinc oxide may be 3 ⁇ m or less.
  • the average particle size (D 50 ) of the aluminum oxide may be 5 ⁇ m or less.
  • the average particle size (D 50 ) of the aluminum nitride may be 5 ⁇ m or less.
  • the silicone composition may further include a colorant.
  • the silicone composition of the present invention has excellent handleability and workability due to good fluidity, and can exhibit excellent heat dissipation due to high thermal conductivity and low contact thermal resistance. Therefore, when the silicone composition of the present invention is applied to a heating element (for example, a computer GPU, a CPU; an ECU in an automotive electric field; a power module of an inverter and an electronic component), heat generated in the heating element is efficiently conducted, thereby The heat dissipation can be improved.
  • a heating element for example, a computer GPU, a CPU; an ECU in an automotive electric field; a power module of an inverter and an electronic component
  • the silicone composition of this invention contains a silicone macromer, a silica, and a filler.
  • Silicone macromers included in the silicone composition of the present invention impart fluidity to the silicone composition to improve the handleability, workability, and the like of the silicone composition.
  • the silicone macromer may have an amount of an alkoxy group bonded to the silicon atom (specifically, the ratio of the alkoxy group to the total functional groups bonded to the silicon atom) of 0.1 to 1 mol%, specifically 0.4 to 0.6 mol%. .
  • the content of the alkoxy group is less than the above range, the viscosity of the silicone composition may be increased or the heat dissipation may be decreased.
  • the alkoxy group is more than the above range, the reliability of the silicone composition may be lowered due to the separation or volatilization of a component having a lower molecular weight. have.
  • the silicone macromer may have a viscosity of 10 to 50 mPa ⁇ s at 25 ° C. in consideration of fluidity of the silicone composition.
  • the viscosity of the silicone macromer is less than 10 mPa ⁇ s, the silicone macromer and the filler may be separated due to the decrease in the mixing property of the silicone macromer and the filler. It is difficult to contain a high content of the silicone composition may lower the heat dissipation.
  • the viscosity of the silicone macromer may be 12 to 42 mPa ⁇ s at 25 ° C., more specifically 22 to 33 mPa ⁇ s.
  • Such a silicone macromer may be a compound represented by the following Chemical Formula 1.
  • n is an integer of 8 to 48. Specifically, n may be an integer of 10 to 40, more specifically may be an integer of 20 to 30.
  • Silica included in the silicone composition of the present invention prevents the silicone macromer from contacting with moisture and improves the durability (mechanical strength) of the silicone composition.
  • the silica may have a specific surface area of 195 to 250 m 2 / g, and may be one that is surface treated with a silazane compound to ensure dispersibility. When the specific surface area of the silica is out of the above range, the dispersibility or flowability of the silica may decrease.
  • hexamethylene disilazane (HMDZ) etc. are mentioned as a specific example of the said silazane compound.
  • the silica content may be 1 to 5 parts by weight, based on 100 parts by weight of the silicone macromer, in consideration of fluidity, heat dissipation, and the like of the silicone composition. If the content of silica is out of the above range, durability or dispersibility may be lowered.
  • the filler included in the silicone composition of the present invention includes two or more selected from the group consisting of zinc oxide, aluminum oxide, and aluminum nitride, and imparts thermal conductivity to the silicone composition to improve heat dissipation of the silicone composition.
  • the silicone composition of the present invention optimizes the particle size of zinc oxide, aluminum oxide, and aluminum nitride used as a filler so that the silicone composition can be made without deteriorating the fluidity of the silicone composition even if the silicone composition contains a high amount of filler. It is possible to lower the contact thermal resistance with the substrate to be applied.
  • the zinc oxide used as the filler may have an average particle size (D 50 ) of 3 ⁇ m or less, and specifically 0.3 to 0.6 ⁇ m. When the average particle size (D 50 ) of zinc oxide is out of the above range, the filling rate of the filler may be lowered.
  • the content of such zinc oxide may be 400 to 900 parts by weight based on 100 parts by weight of the silicone macromer.
  • the heat dissipation of the silicone composition may be lowered.
  • the aluminum oxide used as the filler may have an average particle size (D 50 ) of 5 ⁇ m or less, specifically 3 ⁇ m or less, and may have a spherical shape.
  • D 50 average particle size of the aluminum oxide
  • the thermal resistance of the silicone composition may be lowered.
  • the content of such aluminum oxide may be 400 to 1000 parts by weight based on 100 parts by weight of the silicone macromer.
  • the heat dissipation, workability, etc. of the silicone composition may be lowered.
  • the aluminum nitride used as the filler may have an average particle size (D 50 ) of 5 ⁇ m or less, specifically 1 ⁇ m or less, and the shape may be spherical.
  • D 50 average particle size of the aluminum nitride
  • the content of the aluminum nitride may be 100 to 300 parts by weight based on 100 parts by weight of the silicone macromer. When the content of aluminum nitride is out of the above range, the workability of the silicone composition may be reduced.
  • the silicone composition of the present invention may further include a colorant to adjust the color.
  • the colorant further included in the silicone composition of the present invention imparts color to the silicone composition.
  • the colorant carbon black, aniline black, titanium black, acetylene black, or a mixture thereof may be used.
  • Such a colorant may be 0.5 to 1 part by weight based on 100 parts by weight of the silicone macromer in consideration of color, flowability, heat dissipation, etc. of the silicone composition. If the content of the colorant is outside the above range, the insulation of the silicone composition may be lowered.
  • Such a silicone composition of the present invention may have a viscosity of 10,000 to 70,000 mPa ⁇ s at 25 ° C. As the silicone composition of the present invention exhibits a viscosity within the above range, it is excellent in fluidity and can improve workability such as dispensing property and screen printability.
  • the silicone composition of the present invention has a low thermal resistance and high thermal conductivity of 2.9 W / mK or more, and when applied to a heating element (for example, an electronic product), the heat dissipation of the heating element can be improved.
  • each component was weighed and introduced into a 1 L planetary mixer, followed by mixing at 25 ° C. for 4 hours to prepare a silicone composition.
  • the composition of each component was as shown in Table 1, the content of each component was weighed based on 100 parts by weight of the silicone macromer.
  • the average particle size of the filler was measured using the micro track MT3300EX which is a particle size analyzer from Nikki Kabushiki Kaisha.
  • a silicone composition was prepared through the same process as in Example 1, except that the composition of Table 1 was applied.
  • a silicone composition was manufactured through the same process as in Example 1, except that the composition of Table 2 was applied.
  • Example 1 Example 2 Example 3 Example 4 Example 5 Example 6
  • Example 7 Silicone macromermethoxy group content: 0.5 mol%) 100 100 100 100 100 100 Silicon macromethoxy group content: 1.1 mol%) - - - - - - Silicon macromethoxy group content: 0.05 mol%) - - - - - - - filler Zinc oxide powder (average particle size: 0.6 ⁇ m) 650 550 445 445 445 445 445 Spherical Aluminum Oxide Powder (Average Size: 5 ⁇ m) - - - 610 - - - Spherical Aluminum Oxide Powder (Average Size: 3 ⁇ m) 890 750 610 - 530 650 610 Spherical Aluminum Nitride Powder (Average Particle Size: 1 ⁇ m) - - 260 260 - - - Silica (Specific surface area: 220 m2 / g) 1.6 1.4 1.6 1.3 1.3 1.3 1.3 Toning Agent
  • Comparative Example 1 Comparative Example 2 Silicone macromermethoxy group content: 0.5 mol%) - - Silicon macromethoxy group content: 1.1 mol%) 100 - Silicon macromethoxy group content: 0.05 mol%) - 100 filler Zinc oxide powder (average particle size: 0.6 ⁇ m) 445 445 Spherical Aluminum Oxide Powder (Average Size: 5 ⁇ m) - - Spherical Aluminum Oxide Powder (Average Size: 3 ⁇ m) 610 610 Spherical Aluminum Nitride Powder (Average Particle Size: 1 ⁇ m) - - Silica (Specific surface area: 220 m2 / g) 1.3 1.3 Toning Agent (KCC, YS0108K) 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6
  • Viscosity After leaving the silicone composition in a constant temperature room at 25 ° C. for 24 hours, the viscosity at shear rate 10 was measured using a rheometer viscometer from Brickfield.
  • Thermal Conductivity After injecting the silicone composition into a 3 cm thick mold and covering the kitchen wrap, the thermal conductivity was measured using a thermal conductivity meter (QTM-500) manufactured by Kyoto Denshi Kogyo Co., Ltd.
  • Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 Comparative Example 1 Comparative Example 2 importance 3.5 3.45 3.28 3.3 3.28 3.35 3.33 3.33 3.33 color Gray Gray Gray Gray Gray Gray Gray Gray Gray Gray Gray Gray Gray Gray Gray Gray Gray Gray Gray Gray Gray Gray Gray Gray Gray Gray Gray Gray Gray Viscosity (mPas) 56,000 30,000 65,000 38,000 22,000 50,000 45,000 7,000 25,000 Thermal Conductivity (W / mK) 3.1 2.9 3 3.1 2.2 2.7 2.6 2.5 2.3 Thermal resistance (K / W, thickness: 20 ⁇ m) 0.63 0.64 0.62 0.64 0.66 0.65 0.66 0.66 0.69 Thermal resistance (K / W, thickness: 100 ⁇ m) 0.75 0.75 0.74 0.74 0.76 0.76 0.76 0.76 0.79
  • the silicone composition of the present invention is excellent in thermal conductivity.

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  • Health & Medical Sciences (AREA)
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Abstract

The present invention relates to a silicone composition having excellent heat dissipation properties and being applicable to an electronic product and the like.

Description

방열성이 우수한 실리콘 조성물Silicone composition with excellent heat dissipation
본 발명은 전자 제품의 방열성을 개선하는데 사용되는 실리콘 조성물에 관한 것이다.The present invention relates to silicone compositions used to improve the heat dissipation of electronic products.
전자 제품은 기본적으로 사용 과정에서 열이 발생하는데, 최근의 전자 제품의 경우에는 경량화, 소형화된 반면 많은 양의 정보를 교환하기 때문에 면적 대비 더 많은 열이 발생하고 있다.In general, electronic products generate heat during use. In recent years, electronic products are lighter and smaller, and more heat is generated for an area because they exchange a large amount of information.
따라서, 전자 제품의 성능을 적절히 유지하기 위해서는 전자 제품에서 발생하는 열을 제거하는 것이 필요하다. 특히, 데스크탑, 노트북 등에 사용되고 있는 CPU, GPU 등의 집적회로 소자는 동작 주파수의 고속화에 의해 발열량이 증가하고 있어 방열 대책이 중요한 문제가 되고 있다.Therefore, in order to properly maintain the performance of the electronic product, it is necessary to remove heat generated in the electronic product. In particular, integrated circuit devices such as CPUs and GPUs used in desktops, laptops, and the like have increased heat generation due to higher operating frequencies, so that heat dissipation measures have become an important problem.
상기 전자 제품에서 발생되는 열을 제거하는 방법으로는 다양한 방법이 제안되어 왔는데, 그 중 하나로 전자 제품에 포함된 전자 부품, 히트 싱크 등의 부재 사이에 열전도성 그리스, 열전도성 시트, 열전도성 접착제 등과 같은 열전도성 재료를 마련하여 전자 제품의 방열성을 높인 방법을 들 수 있다.Various methods have been proposed as a method of removing heat generated from the electronic products, and among them, thermally conductive grease, thermally conductive sheets, thermally conductive adhesives, etc., between electronic components and heat sinks included in the electronic products. The method of providing the same thermally conductive material and improving the heat dissipation of an electronic product is mentioned.
이때, 상기 열전도성 재료로는 실리콘 오일에 산화아연 분말, 또는 산화알루미늄 분말과 같은 필러가 배합된 방열 조성물이 알려져 있다. 또한, 실리콘 오일에, 산화아연 분말 및 산화알루미늄 분말과 더불어 다른 필러가 첨가되거나, 열전도성이 높은 다이아몬드, 질화붕소, 탄소나노튜브 등의 필러가 배합된 조성물도 알려져 있다.At this time, as the heat conductive material, a heat dissipating composition in which a filler such as zinc oxide powder or aluminum oxide powder is blended with silicone oil is known. In addition, compositions in which other fillers are added to the silicone oil together with zinc oxide powder and aluminum oxide powder, or fillers such as diamond, boron nitride and carbon nanotubes having high thermal conductivity are also known.
그런데, 이러한 열전도성 재료는 다양한 필러를 포함함에 따라서 전자 제품의 방열성을 개선시킬 수는 있으나, 고함량의 필러로 인해 열전도성 재료의 유동성, 취급성 등이 저하되어 실제적으로 전자 제품에 적용하는데 많은 어려움을 겪고 있다.By the way, the thermally conductive material may improve heat dissipation of electronic products by including various fillers, but due to the high content of fillers, the fluidity and handleability of the thermally conductive material may be deteriorated, and thus many practical applications are applied to electronic products. I'm having a hard time.
[선행기술문헌][Preceding technical literature]
[특허문헌][Patent Documents]
대한민국 공개특허공보 제2004-0059034호Republic of Korea Patent Publication No. 2004-0059034
본 발명은 방열성과 더불어 유동성, 취급성 등이 우수한 실리콘 조성물을 제공하고자 한다.The present invention is to provide a silicone composition having excellent heat dissipation and excellent fluidity, handleability and the like.
본 발명은, 규소 원자에 결합되는 알콕시기의 함량이 0.1 내지 1 mol%인 실리콘 마크로머, 실리카, 및 산화아연, 산화알루미늄 및 질화알루미늄으로 이루어진 군에서 선택된 2종 이상을 포함하는 필러를 포함하는 실리콘 조성물을 제공한다.The present invention comprises a filler comprising a silicon macromer having a content of an alkoxy group bonded to a silicon atom of 0.1 to 1 mol%, silica, and at least two selected from the group consisting of zinc oxide, aluminum oxide and aluminum nitride. Provide a silicone composition.
상기 실리콘 마크로머는 25 ℃에서 점도가 10 내지 50 mPa·s일 수 있다.The silicone macromer may have a viscosity of 10 to 50 mPa · s at 25 ° C.
상기 실리콘 마크로머는 하기 화학식 1로 표시되는 화합물일 수 있다.The silicone macromer may be a compound represented by Formula 1 below.
[화학식 1][Formula 1]
Figure PCTKR2017010010-appb-I000001
Figure PCTKR2017010010-appb-I000001
상기 화학식 1에서, n은 8 내지 48의 정수이다.In Formula 1, n is an integer of 8 to 48.
상기 산화아연(a)과 상기 산화알루미늄(b)과 상기 질화알루미늄(c)의 혼합 비율(a:b:c)은 1: 1.20 내지 1.45: 0 내지 0.6의 중량비일 수 있다.The mixing ratio (a: b: c) of the zinc oxide (a), the aluminum oxide (b) and the aluminum nitride (c) may be a weight ratio of 1: 1.20 to 1.45: 0 to 0.6.
상기 산화아연의 평균 입도(D50)는 3 ㎛ 이하일 수 있다.The average particle size (D 50 ) of the zinc oxide may be 3 μm or less.
상기 산화알루미늄의 평균 입도(D50)는 5 ㎛ 이하일 수 있다.The average particle size (D 50 ) of the aluminum oxide may be 5 μm or less.
상기 질화알루미늄의 평균 입도(D50)는 5 ㎛ 이하일 수 있다.The average particle size (D 50 ) of the aluminum nitride may be 5 μm or less.
상기 실리콘 조성물은 조색제를 더 포함할 수 있다.The silicone composition may further include a colorant.
본 발명의 실리콘 조성물은 양호한 유동성으로 인해 취급성, 작업성이 우수하고, 높은 열전도성 및 낮은 접촉열저항으로 인해 우수한 방열성을 나타낼 수 있다. 따라서, 본 발명의 실리콘 조성물을 발열체(예를 들어, 컴퓨터 GPU, CPU; 자동차 전장의 ECU; 인버터와 전자 부품의 파워모듈 등)에 적용할 경우, 발열체에서 발생된 열이 효율적으로 전도되어 발열체의 방열성을 향상시킬 수 있다.The silicone composition of the present invention has excellent handleability and workability due to good fluidity, and can exhibit excellent heat dissipation due to high thermal conductivity and low contact thermal resistance. Therefore, when the silicone composition of the present invention is applied to a heating element (for example, a computer GPU, a CPU; an ECU in an automotive electric field; a power module of an inverter and an electronic component), heat generated in the heating element is efficiently conducted, thereby The heat dissipation can be improved.
이하, 본 발명을 설명한다.Hereinafter, the present invention will be described.
본 발명의 실리콘 조성물은, 실리콘 마크로머, 실리카, 및 필러를 포함한다.The silicone composition of this invention contains a silicone macromer, a silica, and a filler.
본 발명의 실리콘 조성물에 포함되는 실리콘 마크로머(macromer)는 실리콘 조성물에 유동성을 부여하여 실리콘 조성물의 취급성, 작업성 등을 향상시킨다. 이러한 실리콘 마크로머는 규소 원자에 결합되는 알콕시기의 함량(구체적으로, 규소 원자에 결합된 전체 작용기 중 알콕시기가 차지하는 비율)이 0.1 내지 1 mol%이고, 구체적으로는 0.4 내지 0.6 mol%일 수 있다. 상기 알콕시기의 함량이 상기 범위 미만일 경우에는 실리콘 조성물의 점도가 상승되거나 방열성이 저하될 수 있고, 상기 범위를 초과할 경우에는 분자량이 작은 성분의 분리 또는 휘발로 인해 실리콘 조성물의 신뢰성이 저하될 수 있다.Silicone macromers included in the silicone composition of the present invention impart fluidity to the silicone composition to improve the handleability, workability, and the like of the silicone composition. The silicone macromer may have an amount of an alkoxy group bonded to the silicon atom (specifically, the ratio of the alkoxy group to the total functional groups bonded to the silicon atom) of 0.1 to 1 mol%, specifically 0.4 to 0.6 mol%. . When the content of the alkoxy group is less than the above range, the viscosity of the silicone composition may be increased or the heat dissipation may be decreased. When the alkoxy group is more than the above range, the reliability of the silicone composition may be lowered due to the separation or volatilization of a component having a lower molecular weight. have.
상기 실리콘 마크로머는 실리콘 조성물의 유동성을 고려할 때, 25 ℃에서 점도가 10 내지 50 mPa·s일 수 있다. 상기 실리콘 마크로머의 점도가 10 mPa·s 미만일 경우에는 실리콘 마크로머와 필러의 혼합성 저하로 인해 실리콘 마크로머와 필러가 분리될 수 있으며, 50 mPa·s를 초과할 경우에는 유동성 저하로 인해 필러를 고함량으로 함유하기 어려워 실리콘 조성물의 방열성이 저하될 수 있다. 구체적으로, 실리콘 마크로머의 점도는 25 ℃에서 12 내지 42 mPa·s일 수 있고, 보다 구체적으로는 22 내지 33 mPa·s일 수 있다.The silicone macromer may have a viscosity of 10 to 50 mPa · s at 25 ° C. in consideration of fluidity of the silicone composition. When the viscosity of the silicone macromer is less than 10 mPa · s, the silicone macromer and the filler may be separated due to the decrease in the mixing property of the silicone macromer and the filler. It is difficult to contain a high content of the silicone composition may lower the heat dissipation. Specifically, the viscosity of the silicone macromer may be 12 to 42 mPa · s at 25 ° C., more specifically 22 to 33 mPa · s.
이러한 실리콘 마크로머는 하기 화학식 1로 표시되는 화합물일 수 있다.Such a silicone macromer may be a compound represented by the following Chemical Formula 1.
[화학식 1][Formula 1]
Figure PCTKR2017010010-appb-I000002
Figure PCTKR2017010010-appb-I000002
상기 화학식 1에서, n은 8 내지 48의 정수이다. 구체적으로, n은 10 내지 40의 정수일 수 있고, 보다 구체적으로는 20 내지 30의 정수일 수 있다.In Formula 1, n is an integer of 8 to 48. Specifically, n may be an integer of 10 to 40, more specifically may be an integer of 20 to 30.
본 발명의 실리콘 조성물에 포함되는 실리카는 상기 실리콘 마크로머가 수분과 접촉하는 것을 방지하고 실리콘 조성물의 내구성(기계적 강도)을 향상시킨다. 상기 실리카는 비표면적이 195 내지 250 ㎡/g일 수 있으며, 분산성을 확보하기 위해 실라잔 화합물로 표면처리된 것을 사용할 수 있다. 실리카의 비표면적이 상기 범위를 벗어날 경우, 실리카의 분산성 또는 흐름성이 저하될 수 있다. 한편, 상기 실라잔 화합물의 구체적인 예로는 헥사메틸렌 디실라잔(HMDZ) 등을 들 수 있다.Silica included in the silicone composition of the present invention prevents the silicone macromer from contacting with moisture and improves the durability (mechanical strength) of the silicone composition. The silica may have a specific surface area of 195 to 250 m 2 / g, and may be one that is surface treated with a silazane compound to ensure dispersibility. When the specific surface area of the silica is out of the above range, the dispersibility or flowability of the silica may decrease. In addition, hexamethylene disilazane (HMDZ) etc. are mentioned as a specific example of the said silazane compound.
이러한 실리카의 함량은 실리콘 조성물의 유동성, 방열성 등을 고려할 때, 실리콘 마크로머 100 중량부를 기준으로, 1 내지 5 중량부일 수 있다. 실리카의 함량이 상기 범위를 벗어날 경우, 내구성 또는 분산성이 저하될 수 있다.The silica content may be 1 to 5 parts by weight, based on 100 parts by weight of the silicone macromer, in consideration of fluidity, heat dissipation, and the like of the silicone composition. If the content of silica is out of the above range, durability or dispersibility may be lowered.
본 발명의 실리콘 조성물에 포함되는 필러는 산화아연, 산화알루미늄, 및 질화알루미늄으로 이루어진 군에서 선택된 2종 이상을 포함하는 것으로, 실리콘 조성물에 열전도성을 부여하여 실리콘 조성물의 방열성 등을 향상시킨다.The filler included in the silicone composition of the present invention includes two or more selected from the group consisting of zinc oxide, aluminum oxide, and aluminum nitride, and imparts thermal conductivity to the silicone composition to improve heat dissipation of the silicone composition.
특히, 본 발명의 실리콘 조성물은 필러로 사용되는 산화아연, 산화알루미늄, 및 질화알루미늄의 입자 크기를 최적화하여, 실리콘 조성물에 필러가 고함량으로 함유되더라도 실리콘 조성물의 유동성을 저하시키지 않으면서 실리콘 조성물이 적용되는 기재와의 접촉열저항을 낮출 수 있다.In particular, the silicone composition of the present invention optimizes the particle size of zinc oxide, aluminum oxide, and aluminum nitride used as a filler so that the silicone composition can be made without deteriorating the fluidity of the silicone composition even if the silicone composition contains a high amount of filler. It is possible to lower the contact thermal resistance with the substrate to be applied.
상기 필러로 사용되는 산화아연은 평균 입도(D50)가 3 ㎛ 이하일 수 있고, 구체적으로는 0.3 내지 0.6 ㎛일 수 있다. 산화아연의 평균 입도(D50)가 상기 범위를 벗어날 경우, 필러의 충진율이 저하될 수 있다.The zinc oxide used as the filler may have an average particle size (D 50 ) of 3 μm or less, and specifically 0.3 to 0.6 μm. When the average particle size (D 50 ) of zinc oxide is out of the above range, the filling rate of the filler may be lowered.
이러한 산화아연의 함량은 실리콘 마크로머 100 중량부를 기준으로 400 내지 900 중량부일 수 있다. 산화아연의 함량이 상기 범위를 벗어날 경우, 실리콘 조성물의 방열성이 저하될 수 있다.The content of such zinc oxide may be 400 to 900 parts by weight based on 100 parts by weight of the silicone macromer. When the content of zinc oxide is out of the above range, the heat dissipation of the silicone composition may be lowered.
상기 필러로 사용되는 산화알루미늄은 평균 입도(D50)가 5 ㎛ 이하일 수 있고, 구체적으로는 3 ㎛ 이하일 수 있으며, 형태는 구상일 수 있다. 산화알루미늄의 평균 입도(D50)가 상기 범위를 벗어날 경우, 실리콘 조성물의 열저항성이 저하될 수 있다.The aluminum oxide used as the filler may have an average particle size (D 50 ) of 5 μm or less, specifically 3 μm or less, and may have a spherical shape. When the average particle size (D 50 ) of the aluminum oxide is out of the above range, the thermal resistance of the silicone composition may be lowered.
이러한 산화알루미늄의 함량은 실리콘 마크로머 100 중량부를 기준으로 400 내지 1000 중량부일 수 있다. 산화알루미늄의 함량이 상기 범위를 벗어날 경우, 실리콘 조성물의 방열성, 작업성 등이 저하될 수 있다.The content of such aluminum oxide may be 400 to 1000 parts by weight based on 100 parts by weight of the silicone macromer. When the content of aluminum oxide is out of the above range, the heat dissipation, workability, etc. of the silicone composition may be lowered.
상기 필러로 사용되는 질화알루미늄은 평균 입도(D50)가 5 ㎛ 이하일 수 있고, 구체적으로는 1 ㎛ 이하일 수 있으며, 형태는 구상일 수 있다. 질화알루미늄의 평균 입도(D50)가 상기 범위를 벗어날 경우, 실리콘 조성물의 열저항성이 저하될 수 있다.The aluminum nitride used as the filler may have an average particle size (D 50 ) of 5 μm or less, specifically 1 μm or less, and the shape may be spherical. When the average particle size (D 50 ) of the aluminum nitride is out of the above range, the thermal resistance of the silicon composition may be lowered.
이러한 질화알루미늄의 함량은 실리콘 마크로머 100 중량부를 기준으로 100 내지 300 중량부일 수 있다. 질화알루미늄의 함량이 상기 범위를 벗어날 경우, 실리콘 조성물의 작업성이 저하될 수 있다.The content of the aluminum nitride may be 100 to 300 parts by weight based on 100 parts by weight of the silicone macromer. When the content of aluminum nitride is out of the above range, the workability of the silicone composition may be reduced.
상기 필러로 산화아연(a), 산화알루미늄(b), 및 질화알루미늄(c) 중 2종 이상을 선택하여 혼합할 때, 이들의 혼합 비율(a:b:c)은 1:1.20 내지 1.45:0 내지 0.6의 중량비일 수 있고, 구체적으로는 1:1.30 내지 1.38:0.40 내지 0.6의 중량비일 수 있다. 산화아연, 산화알루미늄, 및 질화알루미늄의 혼합 비율이 상기 범위를 벗어날 경우, 실리콘 조성물의 열전도성 저하로 인해 실리콘 조성물의 방열성이 저하될 수 있다.When two or more of zinc oxide (a), aluminum oxide (b) and aluminum nitride (c) are selected and mixed with the filler, their mixing ratio (a: b: c) is 1: 1.20 to 1.45: It may be a weight ratio of 0 to 0.6, specifically, may be a weight ratio of 1: 1.30 to 1.38: 0.40 to 0.6. When the mixing ratio of zinc oxide, aluminum oxide, and aluminum nitride is out of the above range, the heat dissipation of the silicone composition may be lowered due to a lower thermal conductivity of the silicone composition.
한편, 본 발명의 실리콘 조성물은 색상을 조절하기 위해 조색제를 더 포함할 수 있다.On the other hand, the silicone composition of the present invention may further include a colorant to adjust the color.
본 발명의 실리콘 조성물에 더 포함되는 조색제는 실리콘 조성물에 색상을 부여한다. 상기 조색제로는 카본 블랙, 아닐린 블랙, 티탄 블랙, 아세틸렌 블랙, 또는 이들의 혼합물 등을 사용할 수 있다. 이러한 조색제는 실리콘 조성물의 색상, 유동성, 방열성 등을 고려할 때, 실리콘 마크로머 100 중량부를 기준으로 0.5 내지 1 중량부일 수 있다. 조색제의 함량이 상기 범위를 벗어날 경우, 실리콘 조성물의 절연성이 저하될 수 있다.The colorant further included in the silicone composition of the present invention imparts color to the silicone composition. As the colorant, carbon black, aniline black, titanium black, acetylene black, or a mixture thereof may be used. Such a colorant may be 0.5 to 1 part by weight based on 100 parts by weight of the silicone macromer in consideration of color, flowability, heat dissipation, etc. of the silicone composition. If the content of the colorant is outside the above range, the insulation of the silicone composition may be lowered.
이와 같은 본 발명의 실리콘 조성물은 25 ℃에서 점도가 10,000 내지 70,000 mPa·s일 수 있다. 본 발명의 실리콘 조성물은 상기 범위 내의 점도를 나타냄에 따라 유동성이 우수하여 디스펜스성, 스크린인쇄성 등과 같은 작업성을 높일 수 있다.Such a silicone composition of the present invention may have a viscosity of 10,000 to 70,000 mPa · s at 25 ° C. As the silicone composition of the present invention exhibits a viscosity within the above range, it is excellent in fluidity and can improve workability such as dispensing property and screen printability.
또한, 본 발명의 실리콘 조성물은 열저항이 낮고 열전도도가 2.9 W/mK 이상으로 높은 열전도도를 나타내어, 이를 발열체(예를 들어, 전자 제품)에 적용할 경우 발열체의 방열성을 높일 수 있다.In addition, the silicone composition of the present invention has a low thermal resistance and high thermal conductivity of 2.9 W / mK or more, and when applied to a heating element (for example, an electronic product), the heat dissipation of the heating element can be improved.
이하 본 발명을 실시예를 통하여 상세히 설명하면 다음과 같다. 단, 하기 실시예는 본 발명을 예시하는 것일 뿐, 본 발명이 하기 실시예에 의해 한정되는 것은 아니다.Hereinafter, the present invention will be described in detail with reference to the following Examples. However, the following examples are merely to illustrate the invention, the present invention is not limited by the following examples.
[실시예 1]Example 1
1ℓ의 Planetary mixer에 각 성분을 칭량하여 투입한 후, 25 ℃에서 4 시간 동안 혼합하여 실리콘 조성물을 제조하였다. 이때, 각 성분의 조성은 하기 표 1과 같이 하였으며, 실리콘 마크로머 100 중량부를 기준으로 각 성분의 함량을 칭량하였다. 또한, 필러의 평균 입도는 니끼소 카부시키카이샤의 입도 분석계인 마이크로 트랙 MT3300EX를 이용하여 측정하였다.Each component was weighed and introduced into a 1 L planetary mixer, followed by mixing at 25 ° C. for 4 hours to prepare a silicone composition. At this time, the composition of each component was as shown in Table 1, the content of each component was weighed based on 100 parts by weight of the silicone macromer. In addition, the average particle size of the filler was measured using the micro track MT3300EX which is a particle size analyzer from Nikki Kabushiki Kaisha.
[실시예 2 내지 7][Examples 2 to 7]
하기 표 1의 조성을 적용한 것을 제외하고는 상기 실시예 1과 동일한 과정을 거쳐 실리콘 조성물을 제조하였다.A silicone composition was prepared through the same process as in Example 1, except that the composition of Table 1 was applied.
[비교예 1 및 2][Comparative Examples 1 and 2]
하기 표 2의 조성을 적용한 것을 제외하고는 상기 실시예 1과 동일한 과정을 거쳐 실리콘 조성물을 제조하였다.A silicone composition was manufactured through the same process as in Example 1, except that the composition of Table 2 was applied.
실시예 1Example 1 실시예 2Example 2 실시예 3Example 3 실시예 4Example 4 실시예 5Example 5 실시예 6Example 6 실시예7Example 7
실리콘 마크로머메톡시기 함량: 0.5 mol%)Silicone macromermethoxy group content: 0.5 mol%) 100100 100100 100100 100100 100100 100100 100100
실리콘 마크로머메톡시기 함량: 1.1 mol%)Silicon macromethoxy group content: 1.1 mol%) -- -- -- -- -- -- --
실리콘 마크로머메톡시기 함량: 0.05 mol%)Silicon macromethoxy group content: 0.05 mol%) -- -- -- -- -- -- --
필러filler 산화아연 분말(평균 입도: 0.6 ㎛)Zinc oxide powder (average particle size: 0.6 µm) 650650 550550 445445 445445 445445 445445 445445
구상 산화알루미늄 분말(평균 입도: 5 ㎛)Spherical Aluminum Oxide Powder (Average Size: 5 ㎛) -- -- -- 610610 -- -- --
구상 산화알루미늄 분말(평균 입도: 3 ㎛)Spherical Aluminum Oxide Powder (Average Size: 3 ㎛) 890890 750750 610610 -- 530530 650650 610610
구상 질화알루미늄 분말(평균 입도: 1 ㎛)Spherical Aluminum Nitride Powder (Average Particle Size: 1 ㎛) -- -- 260260 260260 -- -- --
실리카(비표면적: 220 ㎡/g)Silica (Specific surface area: 220 m2 / g) 1.61.6 1.41.4 1.61.6 1.61.6 1.31.3 1.31.3 1.31.3
조색제(KCC, YS0108K)Toning Agent (KCC, YS0108K) 1One 0.80.8 0.60.6 0.60.6 0.60.6 0.60.6 0.60.6
비교예 1Comparative Example 1 비교예 2Comparative Example 2
실리콘 마크로머메톡시기 함량: 0.5 mol%)Silicone macromermethoxy group content: 0.5 mol%) -- --
실리콘 마크로머메톡시기 함량: 1.1 mol%)Silicon macromethoxy group content: 1.1 mol%) 100100 --
실리콘 마크로머메톡시기 함량: 0.05 mol%)Silicon macromethoxy group content: 0.05 mol%) -- 100100
필러filler 산화아연 분말(평균 입도: 0.6 ㎛)Zinc oxide powder (average particle size: 0.6 µm) 445445 445445
구상 산화알루미늄 분말(평균 입도: 5 ㎛)Spherical Aluminum Oxide Powder (Average Size: 5 ㎛) -- --
구상 산화알루미늄 분말(평균 입도: 3 ㎛)Spherical Aluminum Oxide Powder (Average Size: 3 ㎛) 610610 610610
구상 질화알루미늄 분말(평균 입도: 1 ㎛)Spherical Aluminum Nitride Powder (Average Particle Size: 1 ㎛) -- --
실리카(비표면적: 220 ㎡/g)Silica (Specific surface area: 220 m2 / g) 1.31.3 1.31.3
조색제(KCC, YS0108K)Toning Agent (KCC, YS0108K) 0.60.6 0.60.6
[실험예]Experimental Example
제조된 실리콘 조성물의 물성을 하기와 같이 평가하였으며, 그 결과를 하기 표 3에 나타내었다.The physical properties of the prepared silicone composition were evaluated as follows, and the results are shown in Table 3 below.
1. 비중: 비중컵을 이용하여 물의 무게와 실리콘 조성물의 무게를 측정하고, 무게비로 산출하였다.1. Specific gravity: The weight of water and the weight of the silicone composition were measured using a specific gravity cup, and the weight ratio was calculated.
2. 색상: 실리콘 조성물을 육안으로 확인하였다.2. Color: The silicone composition was visually confirmed.
3. 점도: 25 ℃의 항온실에 24 시간 동안 실리콘 조성물을 방치한 후, 브릭필드사의 레오미터 점도계를 이용하여 shear rate 10에서의 점도를 측정하였다.3. Viscosity: After leaving the silicone composition in a constant temperature room at 25 ° C. for 24 hours, the viscosity at shear rate 10 was measured using a rheometer viscometer from Brickfield.
4. 열전도도: 실리콘 조성물을 3 ㎝ 두께의 형틀에 주입하고 키친용 랩을 씌운 후, 교토덴시 공업주식회사의 열전도도계(QTM-500)를 이용하여 열전도도를 측정하였다.4. Thermal Conductivity: After injecting the silicone composition into a 3 cm thick mold and covering the kitchen wrap, the thermal conductivity was measured using a thermal conductivity meter (QTM-500) manufactured by Kyoto Denshi Kogyo Co., Ltd.
5. 열저항: 멘토르 그라픽스사의 T3-ster와 Dyntim 설비의 측정 툴에 실리콘 조성물을 투입한 후, 두께에 따른 열저항을 측정하였다.5. Heat resistance: After the silicone composition was put into the measuring tool of the Mentor Graphix T3-ster and Dyntim equipment, the heat resistance according to the thickness was measured.
실시예 1Example 1 실시예 2Example 2 실시예 3Example 3 실시예 4Example 4 실시예 5Example 5 실시예 6Example 6 실시예7Example 7 비교예 1Comparative Example 1 비교예 2Comparative Example 2
비중importance 3.53.5 3.453.45 3.283.28 3.33.3 3.283.28 3.353.35 3.333.33 3.333.33 3.333.33
색상color GrayGray GrayGray GrayGray GrayGray GrayGray GrayGray GrayGray GrayGray GrayGray
점도(mPa·s)Viscosity (mPas) 56,00056,000 30,00030,000 65,00065,000 38,00038,000 22,00022,000 50,00050,000 45,00045,000 7,0007,000 25,00025,000
열전도도(W/mK)Thermal Conductivity (W / mK) 3.13.1 2.92.9 33 3.13.1 2.22.2 2.72.7 2.62.6 2.52.5 2.32.3
열저항(K/W, 두께: 20 ㎛)Thermal resistance (K / W, thickness: 20 ㎛) 0.630.63 0.640.64 0.620.62 0.640.64 0.660.66 0.650.65 0.660.66 0.660.66 0.690.69
열저항(K/W, 두께: 100 ㎛)Thermal resistance (K / W, thickness: 100 ㎛) 0.750.75 0.750.75 0.740.74 0.740.74 0.760.76 0.760.76 0.760.76 0.760.76 0.790.79
상기 표 3을 참조하면, 본 발명의 실리콘 조성물은 열전도도가 우수한 것을 확인할 수 있다.Referring to Table 3, it can be confirmed that the silicone composition of the present invention is excellent in thermal conductivity.

Claims (8)

  1. 규소 원자에 결합되는 알콕시기의 함량이 0.1 내지 1 mol%인 실리콘 마크로머,Silicone macromers having an alkoxy group bonded to a silicon atom in an amount of 0.1 to 1 mol%,
    실리카, 및Silica, and
    산화아연, 산화알루미늄, 및 질화알루미늄으로 이루어진 군에서 선택된 2종 이상을 포함하는 필러를 포함하는 실리콘 조성물.A silicon composition comprising a filler comprising at least two selected from the group consisting of zinc oxide, aluminum oxide, and aluminum nitride.
  2. 청구항 1에 있어서,The method according to claim 1,
    상기 실리콘 마크로머는 25 ℃에서 점도가 10 내지 50 mPa·s인 것인 실리콘 조성물.The silicone macromer has a viscosity of 10 to 50 mPa · s at 25 ° C.
  3. 청구항 1에 있어서,The method according to claim 1,
    상기 실리콘 마크로머가 하기 화학식 1로 표시되는 화합물인 것인 실리콘 조성물.Silicone composition, wherein the silicone macromer is a compound represented by the following formula (1).
    [화학식 1][Formula 1]
    Figure PCTKR2017010010-appb-I000003
    Figure PCTKR2017010010-appb-I000003
    상기 화학식 1에서,In Chemical Formula 1,
    n은 8 내지 48의 정수이다.n is an integer from 8 to 48.
  4. 청구항 1에 있어서,The method according to claim 1,
    상기 산화아연(a)과 상기 산화알루미늄(b)과 상기 질화알루미늄(c)의 혼합 비율(a:b:c)이 1: 1.20 내지 1.45: 0 내지 0.6의 중량비인 것인 실리콘 조성물.The silicon composition of the zinc oxide (a), the aluminum oxide (b) and the aluminum nitride (c) is a mixing ratio (a: b: c) of 1: 1.20 to 1.45: 0 to 0.6 by weight.
  5. 청구항 1에 있어서,The method according to claim 1,
    상기 산화아연의 평균 입도(D50)가 3 ㎛ 이하인 것인 실리콘 조성물.Silicone composition, wherein the average particle size (D 50 ) of the zinc oxide is 3 ㎛ or less.
  6. 청구항 1에 있어서,The method according to claim 1,
    상기 산화알루미늄의 평균 입도(D50)가 5 ㎛ 이하인 것인 실리콘 조성물.Silicone composition, wherein the average particle size (D 50 ) of the aluminum oxide is 5 ㎛ or less.
  7. 청구항 1에 있어서,The method according to claim 1,
    상기 질화알루미늄의 평균 입도(D50)가 5 ㎛ 이하인 것인 실리콘 조성물.The silicon composition of which the average particle size (D 50 ) of the aluminum nitride is 5 μm or less.
  8. 청구항 1에 있어서,The method according to claim 1,
    조색제를 더 포함하는 것인 실리콘 조성물.Silicone composition further comprising a colorant.
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