KR20160016982A - Boronnitride dispersion composition using a polyamic acid as a dispersing agent - Google Patents

Boronnitride dispersion composition using a polyamic acid as a dispersing agent Download PDF

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KR20160016982A
KR20160016982A KR1020160007407A KR20160007407A KR20160016982A KR 20160016982 A KR20160016982 A KR 20160016982A KR 1020160007407 A KR1020160007407 A KR 1020160007407A KR 20160007407 A KR20160007407 A KR 20160007407A KR 20160016982 A KR20160016982 A KR 20160016982A
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polyamic acid
boron nitride
dispersion
dianhydride
dispersion composition
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김윤구
이길성
손호석
이용석
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에스엠에스주식회사
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Abstract

The present invention relates to a composition and manufacturing of a boron nitride dispersion having heat radiation property. More particularly, the present invention relates to a manufacturing method of a material which uses boron nitride as a heat radiating material, and has excellent surface smoothness and heat radiation property by applying polyamic acid as a dispersing agent and dispersing the composition. The boron nitride dispersion composition for heat radiation comprises: 10 to 50 wt% of boron nitride; 1.0 to 10 wt% of polyamic acid; and 30 to 80 wt% of a solvent.

Description

폴리아믹산을 분산제로 사용하는 방열용 질화붕소 분산액 조성물 {Boronnitride dispersion composition using a polyamic acid as a dispersing agent}[0001] The present invention relates to a boron nitride dispersion composition using a polyamic acid as a dispersing agent,

플렉서블 디스플레이란 플라스틱등 유연한 재료를 사용하여 기능의 손실없이 자유롭게 구부리거나, 두루말이처럼 말거나 접을 수 있는 형태의 디스플레이를 말한다.Flexible display refers to a display that can be flexibly bent, rolled or folded without loss of function using flexible materials such as plastic.

스마트폰, 곡면TV, 스마트워치 등의 등장으로 플렉서블디스플레이가 주목받고 있다.Flexible displays are attracting attention due to the emergence of smartphones, surface TVs, and smart watches.

플렉서블 디스플레이를 구현하기 위해서는 다양한 요소 기술이 필요하며 기판기술, 구동소자 기술, 디스플레이모드 기술, 공정기술이 핵심적인 기술이다.In order to realize flexible display, various element technologies are required, and substrate technology, driving device technology, display mode technology, and process technology are key technologies.

특히 기판의 경우 기존 유리형태의 단단한 기판을 유연한 소재로 전환하면서도 LCD나 OLED와 동등한 화질을 구현하는데 있어 핵심이 되는 재료이다. In particular, substrates are key materials for achieving the same image quality as LCDs and OLEDs, while converting existing glass-type rigid substrates into flexible materials.

PI(Polyimide), FRP(Fiber Reinforced Plastic), PC(Polycarbonate), PET(Polyethyleneterephtalate),PES(Polyethersulfone),PEN(Polyethylenenaphthalate), Metal Foil등 다양한 재료가 검토되고 있으며, 이 중 유력한 재료로서 PI(Polyimide), FRP(Fiber Reinforced Plastic)가 가장 부각되고 있다.Various materials such as PI (Polyimide), FRP (Fiber Reinforced Plastic), PC (Polycarbonate), PET (Polyethyleneterephtalate), PES (Polyethersulfone), PEN (Polyethylenaphthalate) and Metal Foil have been studied. ) And FRP (Fiber Reinforced Plastic).

특히 PI의 경우 우수한 내화학성, 내열성, 절연성의 장점을 가지고 있는 재료로서 플렉서블 기판소재로 가장 활발하게 검토가 진행되고 있다.Particularly, PI is one of the most favorable materials for flexible substrate materials because it has the advantages of excellent chemical resistance, heat resistance and insulation.

본 발명은 플랙서블 기판재료와 혼용함으로서 방열성 및 열안정성을 부여하는 것을 목적으로 하는 제품에 관한 것이다. The present invention relates to a product aimed at imparting heat radiation and thermal stability by being mixed with a flexible substrate material.

최근 각종 전자기기의 고성능화, 소형화 및 고기능화에 따라 전자부품에서의 발열량이 증가함에 따라 기기의내부온도가 상승하여 반도체 소자의 오작동, 저항체 부품의 특성변화 및 부품의 수명이 저하되는 문제를 수반한다. 이러한 문제점을 해결하기 위한 방열대책으로 다양한 기술이 적용되고 있다.In recent years, with the increase in the performance, the miniaturization and the high performance of various electronic devices, the internal temperature of the device rises as the amount of heat generated by the electronic components increases, thereby causing malfunctioning of the semiconductor devices, changes in characteristics of the resistor parts and lifetime of the parts. Various techniques have been applied to solve such a problem.

신소재 세라믹에서 기계가공성이 뛰어난 보론나이트라이드(이하 BN)는 흑연과 비슷한 6방정계 구조를 갖고 있어 화학적 물리적 성질이 흑연과 비슷하다. 그러나 두 물질간에는 다소 중요한 차이가 있는데, BN은 백색으로서 전기적으로 뛰어난 절연체이고 흑연은 전기적으로 도체이다.Boron nitride (hereinafter referred to as BN), which has excellent machinability in new materials ceramics, has a hexavalent structure similar to that of graphite, and its chemical and physical properties are similar to those of graphite. However, there is a somewhat significant difference between the two materials: BN is white, an electrically superior insulator, and graphite is an electrically conductive material.

BN은 불활성 분위기에서는 최대 3000도까지 안정하고 이 온도에서는 승화되기 때문에 연화되는 일은 없다. 스텐레스 스틸정도의 높은 열전도율이 있어 열충격저항이 크고 1500도 정도의 급가열 급냉각을 반복하여도 균열이나 파손되지 않는다.BN is stable up to 3000 degrees in an inert atmosphere and is not softened because it sublimes at this temperature. It has a high thermal conductivity as high as that of stainless steel, so it has a high thermal shock resistance and does not crack or break even if it is repeatedly cooled to about 1500 degrees.

BN의 전기저항값은 고밀도의 고순도 알루미나 세라믹에 비하여 월등히 높다. 특히 고온에서의 변화값이 적어 넓은 온도 범위에서 전기절연재료로 사용된다. The electrical resistivity of BN is much higher than that of high density alumina ceramics. Particularly, it is used as an electrical insulating material in a wide temperature range because the change value at a high temperature is small.

BN은 대부분의 유기용매에 내식성이 우수하다. 또한, 금, 은, 동, 철, 알루미늄, 아연, 납, 주석, 니켈, 망간, 게르마늄, 갈륨, 실리콘, 유리등의 용융물과의 반응성도 없어 화학적안정성이 우수하다.BN is superior in corrosion resistance to most organic solvents. In addition, there is no reactivity with melts such as gold, silver, copper, iron, aluminum, zinc, lead, tin, nickel, manganese, germanium, gallium, silicon and glass.

BN은 세라믹 가공에서 유일하게 다이아몬드공구가 필요 없으며 보통의 금속가공과 같이 공작기계로 복잡한 형상가공이 가능합니다. 또한 진비중이 2.26으로 쎄라믹스 중에서는 가장 가벼워 항공기 우주재료의 부품 경량화에 최적의 재료이다. BN is the only ceramic processing tool that does not require a diamond tool. In addition, the true specific gravity is 2.26, which is the lightest among the ceramics, making it the most suitable material to lighten the parts of aerospace materials.

구부릴 수 있는 디스플레이나 전자종이, 착용식 컴퓨터(wearable computer) 등을 만들 때 적용되는 폴리이미드등의 재료에 평탄도를 가지면서, 열적안정성 및 방열특성을 나타내는 재료에 대한 필요성이 꾸준히 제기되었다.There is a continuing need for materials that exhibit thermal stability and heat dissipation properties while having flatness in materials such as bendable displays, electronic paper, and wearable computers.

본 발명은 방열특성을 갖는 질화붕소 분산액의 조성물 및 제조에 관한 것으로서, 구체적으로 질화붕소를 방열재료로 사용하고 분산제로서 폴리아믹산을 적용하여 분산시킴으로서 평탄성 및 방열특성이 우수한 재료를 제조하는 방법에 관한 것이다.More particularly, the present invention relates to a method for producing a material having excellent flatness and heat dissipation properties by using boron nitride as a heat radiation material and polyamic acid as a dispersant to disperse the composition. will be.

본 발명의 방열용 질화붕소 조성물은, 1.0중량% 내지 50중량%의 질화붕소, 1.0% 내지 10중량%의 폴리아믹산, 30중량% 내지 80중량% 용매를 포함한다.The heat-dissipating boron nitride composition of the present invention comprises 1.0 wt% to 50 wt% boron nitride, 1.0 wt% to 10 wt% polyamic acid, and 30 wt% to 80 wt% solvent.

이 때, 평균입자경이 1 내지 200 nm인 도전성 필러가 1 내지 50중량%가 더 포함될 수 있다.In this case, the conductive filler having an average particle size of 1 to 200 nm may be further contained in an amount of 1 to 50% by weight.

또한, 상기 폴리아믹산은 , 1.0% 내지 10중량%을 포함될 수 있다.In addition, the polyamic acid may include 1.0% to 10% by weight.

또한, 상기 용매는 N-메틸피롤리돈(N-methylpyrrolidone), 디메틸아세트아미드(dimethylacetamide), 디아민(diamine), 디안하이드라이드(dianhydride), 디메틸포름아미드(dimethylformamide), 디메틸 술폭시드 (dimethyl sulfoxide)로 이루어진 군에서 선택되는 1종 또는 2종이상의 혼합물이 사용될 수 있다.The solvent may be selected from the group consisting of N-methylpyrrolidone, dimethylacetamide, diamine, dianhydride, dimethylformamide, dimethyl sulfoxide, Or a mixture of two or more of them may be used.

분산의 과정을 살펴보면 용매와 혼합된 바인더가 필러와 혼합 믹싱하는 젖음 단계;In the course of dispersion, a wetting step in which a binder mixed with a solvent mixes with a filler;

고속 교반기를 사용하여 행하는 1차 분산 단계; 및 상기 1차 분산 단계 후에 밀장비를 사용하여 분산하는 2차 분산 단계 초음파를 사용하여 분산액을 안정시키는 안정단계를 포함하여 제조될 수 있다.A primary dispersion step performed using a high-speed stirrer; And a stabilization step of stabilizing the dispersion using a secondary dispersion step ultrasonic wave which is dispersed using the mill equipment after the primary dispersion step.

또한, 상기 2차 분산단계에서 분산온도는 60℃이하인 것이 바람직하다.The dispersion temperature in the secondary dispersion step is preferably 60 占 폚 or lower.

또한, 분산제, 침강방지제, 소포제, 레벨링제로 이루어진 군에서 선택된 1종 이상의 첨가제를 2 내지 5 중량%로 더 포함할 수 있다.Further, it may further comprise 2 to 5% by weight of at least one additive selected from the group consisting of a dispersing agent, an anti-settling agent, a defoaming agent and a leveling agent.

본 발명에 따른 방열용 질화붕소 분산액 조성물은 기판소재인 PI, FRP등의 재료에 첨가되어 열효율을 크게 하여 플렉서블 기판재료의 냉각 효율을 향상시키고, 열 배출 문제를 효과적으로 해결함으로써, 부품의 작동에 따라 발생되는 열을 기판 자체에서 분산시켜주는 효과가 있다.The boron nitride dispersion composition for heat radiation according to the present invention is added to materials such as PI and FRP as substrate materials to increase the thermal efficiency to improve the cooling efficiency of the flexible substrate material and effectively solve the heat discharge problem, The generated heat is dispersed in the substrate itself.

도 1은 본 발명의 일실시예에 따라 사용된 BN의 TEM 사진.
도 2는 본 발명의 일실시예에 따라 사용된 BN의 TGA 도면.
1 is a TEM photograph of a BN used in accordance with an embodiment of the present invention.
2 is a TGA drawing of a BN used in accordance with an embodiment of the present invention.

이하, 첨부된 도면을 참조하면서 본 발명의 실시예에 따른 방열용 질화붕소 분산액 조성물을 설명한다.BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, a heat-dissipating boron nitride dispersion composition according to an embodiment of the present invention will be described with reference to the accompanying drawings.

본 발명에 따른 방열용 질화붕소 분산액 조성물은 폴리아믹산, 질화붕소 파우더, 및 용매를 포함한다.The heat-dissipating boron nitride dispersion composition according to the present invention comprises a polyamic acid, a boron nitride powder, and a solvent.

본발명에서 사용되는 질화붕소(BN : Boron Nitride, 이하 “BN" 이라 함)은 절연 특성을 갖는 세라믹이면서도 금속과 유사한 열전도 특성을 갖는 비산화물계 세라믹이다. Boron nitride (BN) used in the present invention is a non-oxide ceramics having a thermal conductivity similar to that of a metal, while being a ceramic having an insulating property.

BN는 우수한 윤활성, 화학적안정성, 높은 열전도성과 방열성, 전기절연성 등의 특징을 가지고 있는 소재이다. BN is a material that has excellent lubricity, chemical stability, high thermal conductivity, heat dissipation, and electrical insulation.

BN은 윤활유, 그리스, 물, 용제등에 분산시켜 윤활제의 첨가제로 사용할 수 있으며, 강력한 열저항성을 이용하여 고온 윤활용 첨가제로 사용할 수 있다. 또한 높은 절연파괴강도와 저항성을 가지고 있으므로, 전기절연체로 활용할 수 있다. 반도체 기판, 전자레인지의 투명 유리창, 연료전지와 배터리 전극과 촉매, 밀봉제 등과 같은 전자산업의 전기절연체로 사용되며 절연과 방열을 위한 충전재료도 이용된다. BN can be used as an additive for lubricant by dispersing it in lubricating oil, grease, water, solvent, etc., and can be used as a high temperature lubricant additive due to its strong heat resistance. It also has high dielectric breakdown strength and resistance, so it can be used as an electrical insulator. It is used as an electrical insulator in the electronic industry such as semiconductor substrates, transparent glass windows in microwave ovens, fuel cells and battery electrodes and catalysts, encapsulants, etc., and filling materials for insulation and heat dissipation are also used.

BN은 화학적으로 안정하기 때문에, 도가니, 선박, 용융금속 운송 배관, 펌프, 연전쌍 보호전선외피, 반응기의 내벽에도 적용할 수 있다. 열전도성이 우수하기 때문에 다양한 형태의 방열 첨가제로 활용되고있다. Because BN is chemically stable, it can also be applied to crucibles, ships, molten metal transport piping, pumps, protective jackets of twinning pairs, and inner walls of reactors. Because of its excellent thermal conductivity, it has been utilized as various types of heat radiation additives.

본발명에서 사용되는 분산제로 채용한 폴리아믹산은, 열이나 촉매에 의해 폴리이미드를 형성한다. 아민가와 산가를 모두 가지므로 분산제로서도 사용이 가능하다. 또한 고투명성을 나타내면서도 내열성이 우수하고 낮은 열팽창계수를 가진다.The polyamic acid employed as the dispersant used in the present invention forms a polyimide by heat or a catalyst. It can also be used as a dispersant since it has both amine value and acid value. It exhibits high transparency while exhibiting excellent heat resistance and a low thermal expansion coefficient.

폴리아믹산용액은 디안하이드라이드와 디아민 및 유기용매를 사용하여 합성된다.The polyamic acid solution is synthesized using dianhydride, diamine and organic solvent.

상기 사용되는 디안하이드라이드 는 방향족 디안하이드라이드라면 별히 한정되지 않는다. 예를 들어, 피로멜리틱 디안하이드라이드 (pyromellitic dianhydride, PMDA), 3,3',4,4'-비페닐테트라카르복실릭 디안하이드라이드 (3,3'4,4'-biphenyltetracarboxylic acid dianhydride, BPDA),3,3',4,4'-벤조페논테트라카르복실릭 디안하이드라이드 (3,3',4,4'-benzophenonetetracarboxylic dianhydride,TDA), 4,4'옥시다이프탈릭 안하이드라이드 (4,4′-oxydiphthalic anhydride, ODPA), 2,2-비스[4-3,4-디카르복시페녹시] 페닐]프로판 디안하이드라이드 (2,2-Bis[4-(3,4-dicarboxyphenoxy) phenyl]propane dianhydride,BPADA), 에틸렌 글리콜 비스(4-트리멜리테이트 안하이드라이드 (ethylene glycol bis(4-trimellitateanhydride), TMEG) 등이 있는데, 이에 한정되지 않는다. 이들은 단독으로 또는 2종 이상이 혼합되어 사용될 수 있다. The dianhydride used is not particularly limited as long as it is an aromatic dianhydride. For example, pyromellitic dianhydride (PMDA), 3,3 ', 4,4'-biphenyltetracarboxylic acid dianhydride (3,3'4,4'-biphenyltetracarboxylic acid dianhydride, BPDA), 3,3 ', 4,4'-benzophenone tetracarboxylic dianhydride (TDA), 4,4'oxydiphthalic anhydride (4,4'-oxydiphthalic anhydride, ODPA), 2,2-bis [4-3,4-dicarboxyphenoxy] phenyl] propanediamine hydride ) phenyl] propane dianhydride (BPADA), ethylene glycol bis (4-trimellitate anhydride), TMEG), and the like. Can be mixed and used.

본 발명에서 사용된 폴리아믹산 용액은 방향족 디아민이라면,특별히 한정되지 않는다.The polyamic acid solution used in the present invention is not particularly limited as long as it is an aromatic diamine.

예를 들어, 불소화 디아민의 경우 2,2'-비스(트리플루오로메틸)-4,4'-디아미노비페닐 (2,2'-Bis(trifluoromethyl) -4,4'-Diaminobiphenyl, 2,2'-TFDB), 비스 아미노하이드록시 페닐 헥사플르오로프로판 (bisaminohydroxyphebylhexafluoropropane, DBOH), 비스 아미노페녹시 페닐 헥사플루오로프로판 (bis aminophenoxy phenylhexafluoropropane, 4BDAF), 2,2'-비스(트리플루오로메틸)-4,3'-디아미노비페닐 (2,2'-Bis(trifluoromethyl)-4,3'-Diaminobiphenyl), 2,2'-비스(트리플루오로메틸)-5,5'-디아미노비페닐 (2,2'-Bis(trifluoromethyl)-5,5'-Diaminobiphenyl) 등이 있는데, 이에 한정되지 않는다. 이들은 단독으로 또는 2종 이상이 혼합되어 사용될 수 있다For example, in the case of a fluorinated diamine, 2,2'-bis (trifluoromethyl) -4,4'-diaminobiphenyl (2,2'-bis (trifluoromethyl) 2'-TFDB), bisaminohydroxyphebylhexafluoropropane (DBOH), bisaminophenoxy phenylhexafluoropropane (4BDAF), 2,2'-bis (trifluoromethyl) -4,3'-diaminobiphenyl, 2,2'-bis (trifluoromethyl) -5,5'-diaminobiphenyl, Phenyl (2,2'-bis (trifluoromethyl) -5,5'-diaminobiphenyl), but are not limited thereto. These may be used alone or in combination of two or more thereof

선택적으로, 본 발명의 폴리아믹산 용액은 방향족 디아민 성분으로 m-페닐렌디아민 이외 다른 비-불소화 방향족 디아민을 더 포함할 수 있다. 상기 비-불소화 방향족 디아민의 비제한적인 예로는 p-페닐렌디아민(p-PDA), 옥시디아닐린(ODA), m-메틸렌디아민(m-MDA), 비스 아미노 페녹시 페닐프로판(6HMDA), 비스 아미노페녹시 디페닐술폰(DBSDA) 등이 있는데, 이들은 단독으로 또는 2종 이상이 혼합되어 사용될 수 있다.Optionally, the polyamic acid solution of the present invention may further comprise non-fluorinated aromatic diamines other than m-phenylenediamine as the aromatic diamine component. Non-limiting examples of such non-fluorinated aromatic diamines include p-phenylenediamine (p-PDA), oxydianiline (ODA), m-methylenediamine (m-MDA), bisaminophenoxyphenylpropane (6HMDA) Bisaminophenoxy diphenyl sulfone (DBSDA), etc. These may be used alone or in admixture of two or more.

본 발명의 폴리아믹산 용액에서, 상기 방향족 디안하이드라이드와 방향족 디아민의 몰수비는 특별히 한정되지 않으나, [디안하이드라이드/디아민]이 0.9~1.1, 바람직하게는 0.95~1일경우, 폴리아믹산 용액의 점도가 약 10내지 500 cps로 조절되어, 분산제로서 사용하기에 적합하다In the polyamic acid solution of the present invention, the molar ratio of the aromatic dianhydride to the aromatic diamine is not particularly limited. When the [dianhydride / diamine] is 0.9-1.1, preferably 0.95-1, the polyamic acid solution The viscosity is adjusted to about 10 to 500 cps and is suitable for use as a dispersant

본 발명에서 사용 가능한 유기 용매는 당 업계에 공지된 것이라면 특별히 한정되지 않는다. 예를 들어, m-크레졸, N-메틸-2-피롤리돈(NMP), N,N-디메틸포름아미드(DMF), 디메틸아세트아미드(DMAc), 디메틸설폭사이드(DMSO), 아세톤, 디에틸아세테이트 등과 같은 극성용매를 사용할 수 있다. 이외, 테트라하이드로퓨란(THF), 클로로포름 등과 같은 저비점 용액 또는 γ-부티로락톤과 같은 저흡수성 용매를 사용할 수 있다.The organic solvent usable in the present invention is not particularly limited as long as it is known in the art. (DMF), dimethylacetamide (DMAc), dimethylsulfoxide (DMSO), acetone, diethyl (N, N-dimethylformamide A polar solvent such as acetate may be used. In addition, a low boiling point solution such as tetrahydrofuran (THF), chloroform or the like or a low absorption solvent such as gamma -butyrolactone may be used.

전술한 본 발명의 폴리아믹산 용액에서 방향족 디안하이드라이드, 방향족 디아민 및 유기용매의 함량은 특별히 한정되지 않는다.The content of the aromatic dianhydride, the aromatic diamine and the organic solvent in the polyamic acid solution of the present invention is not particularly limited.

(폴리아믹산의 합성)(Synthesis of polyamic acid)

합성예 1Synthesis Example 1

교반기, 온도조절장치, 질소주입장치, 적하깔대기 및 냉각기를 부착한 1L의 반응기에 질소가스를 서서히 통과시키면서 2,2”-Bis(Trifluoromethyl)biphenyl-4,4”-diamine 17.85g(0.056mole)와 반응용매 NMP 270g을 넣은 후 녹을 때까지 교반한다. 완전히 용해되면 고체상의 Pyromelitic dianhydride 12.15g(0.056mole)을 서서히 첨가하였다. 이 때 고형분 농도는 10중량%로 고정하였으며, 반응온도 25℃에서 10시간 반응시켰다. 고유점도를 측정하였고 그 결과를 표 1에 나타내었다.17.55 g (0.056 mole) of 2,2 " -Bis (Trifluoromethyl) biphenyl-4,4 " -diamine was slowly added to a 1 L reactor equipped with a stirrer, a temperature controller, a nitrogen inlet, a dropping funnel and a condenser, And 270 g of a reaction solvent NMP, and the mixture is stirred until it is dissolved. When completely dissolved, 12.15 g (0.056 mole) of solid phase pyromelitic dianhydride was slowly added. At this time, the solid concentration was fixed at 10% by weight, and the reaction was carried out at a reaction temperature of 25 캜 for 10 hours. The intrinsic viscosity was measured and the results are shown in Table 1.

합성예 2Synthesis Example 2

산무수물로 PBTA 17.55g(0.056mole)로 변경한 것을 제외하고는 합성예 1과 동일하게 실시하여 그 결과를 표 1에 나타내었다.The results are shown in Table 1, except that the amount of the acid anhydride was changed to 17.55 g (0.056 mole) of PBTA.

합성예 3Synthesis Example 3

디아민을 4,4-OXYDIANILINE 11.49g(0.057mole), 디안하이드라이드를 BENZOPHENONE-3, 3', 4, 4'-TETRACARBOXYLIC DIANHYDRIDE 18.51g(0.057mole)로 변경한 것을 제외하고는 합성예 1과 동일하게 실시하여 그 결과를 표 1에 나타내었다.Diamine was changed to 11.49 g (0.057 mole) of 4,4-OXydianiline, and the dianhydride was changed to 18.51 g (0.057 mole) of BENZOPHENONE-3, 3 ', 4,4'-tetracarboxylanic dianhydride The results are shown in Table 1. < tb > < TABLE >

합성예 4Synthesis Example 4

디아민을 (2,2''-BIS(TRIFLUOROMETHYL)BIPHENYL-4,4''-DIAMINE 14.95g(0.047mole), 디안하이드라이드를 BENZOPHENONE-3, 3', 4, 4'-TETRACARBOXYLIC DIANHYDRIDE 15.05g(0.047mole)로 변경한 것을 제외하고는 합성예 1과 동일하게 실시하여 그 결과를 표 1에 나타내었다.Diamine was added to a solution containing 14.95 g (0.047 mole) of bis (2, 2 " -BIS (TRIFLUOROMETHYL) BIPHENYL-4, 4 "- DIAMINE, 15.05 g of dienhydride BENZOPHENONE-3, 3 ', 4, 4'-TETRACARBOXYLIC DIANHYDRIDE 0.047 mole) in the same manner as in Synthesis Example 1. The results are shown in Table 1. < tb > < TABLE >

합성예 5Synthesis Example 5

디아민을 4,4-OXYDIANILINE 14.36g(0.045mole), 디안하이드라이드를 PYROMELITIC DIANHYDRIDE 15.64g(0.045mole)로 변경한 것을 제외하고는 합성예 1과 동일하게 실시하여 그 결과를 표 1에 나타내었다.The diamine was changed to 14.36 g (0.045 mole) of 4,4-OXydianiline, and the dianhydride was changed to 15.64 g (0.045 mole) of PYROMELITIC DIANHYDRIDE. The results are shown in Table 1.

점도(cps)Viscosity (cps) 색상color 폴리아믹산 1Polyamic acid 1 1515 무색투명transparent 폴리아믹산 2Polyamic acid 2 3535 무색투명transparent 폴리아믹산 3Polyamic acid 3 8383 황적색투명Yellowish red transparent 폴리아믹산 4Polyamic acid 4 7070 황적색투명Yellowish red transparent 폴리아믹산 5Polyamic acid 5 5555 황적색투명Yellowish red transparent

표 1에서의 점도는 점도계(Brookfield 점도계, DV-2+)를 사용하여 측정한 값이다. The viscosity in Table 1 is a value measured using a viscometer (Brookfield viscometer, DV-2 +).

(질화붕소 분산액의 제조)(Preparation of Boron Nitride Dispersion)

(실시예 1)(Example 1)

분산액Dispersion [g][g] 질화붕소Boron nitride 2020 폴리아믹산 1Polyamic acid 1 2020 NMPNMP 5858 분산제Dispersant 00 system 100100

상기 표 2에 기재된 조성을 모두 혼합한 후, ASADA社의 Pico mill을 사용하여 6시간 동안 분산을 실시한 후 초음파(CMT Technology, 일본, 500W, 40KHz)를 1시간 처리하여 질화알미늄 분산액을 제조하였다.After all of the compositions shown in Table 2 were mixed, the mixture was dispersed for 6 hours using a Pico mill manufactured by ASADA, and treated with ultrasonic waves (CMT Technology, Japan, 500 W, 40 KHz) for 1 hour to prepare an aluminum nitride dispersion.

(실시예2)(Example 2)

상기 표2에서 폴리아믹산 2로 변경한 것을 제외하고는 실시예1과 동일하게 제조하였다.The procedure of Example 1 was repeated except that the polyamic acid 2 was changed to the polyamic acid 2 in the above Table 2.

(실시예3)(Example 3)

상기 표2에서 폴리아믹산 3으로 변경한 것을 제외하고는 실시예1과 동일하게 제조하였다.The procedure of Example 1 was repeated except that polyamic acid 3 was changed to polyamic acid 3 in Table 2.

(제조예4)(Production Example 4)

상기 표2에서 폴리아믹산 4로 변경한 것을 제외하고는 실시예1과 동일하게 제조하였다.The procedure of Example 1 was repeated except that the polyamic acid 4 was changed to the polyamic acid 4 in the above Table 2.

(제조예5)(Production Example 5)

상기 표2에서 폴리아믹산 4로 변경한 것을 제외하고는 실시예1과 동일하게 제조하였다.The procedure of Example 1 was repeated except that the polyamic acid 4 was changed to the polyamic acid 4 in the above Table 2.

(비교예1)(Comparative Example 1)

상기 표2에서 분산제를 DISPERBYK-111을 2% 추가한 것을 제외하고는 실시예1과 동일하게 제조하였다.In Table 2, DISPERBYK-111 was added in an amount of 2% as a dispersant.

(비교예2)(Comparative Example 2)

상기 표2에서 분산제를 DISPERBYK-110을 2% 추가한 것을 제외하고는 실시예1과 동일하게 제조하였다.In Table 2, DISPERBYK-110 was added in an amount of 2% as a dispersant.

(비교예3)(Comparative Example 3)

상기 표2에서 분산제를 BYK-2001을 2% 추가한 것을 제외하고는 실시예1과 동일하게 제조하였다.The dispersant was prepared in the same manner as in Example 1 except that 2% of BYK-2001 was added as a dispersant in Table 2 above.

분산 직후Immediately after dispersion 분산 후 7일경화7 days hardening after dispersion 분산 후 30일 경과30 days after dispersion 폴리아믹산과의 상용성Compatibility with polyamic acids 실시예1Example 1 층분리Layer separation 침전 후 cakingCaking after precipitation 층분리 후 cakingCaking after layer separation 층분리Layer separation 실시예2Example 2 분산불량Poor dispersion 분산불량Poor dispersion cakingcaking CakingCaking 실시예3Example 3 양호Good 양호Good 양호Good 양호Good 실시예4Example 4 양호Good 양호Good 양호Good 양호Good 실시예5Example 5 양호Good 양호Good 양호Good 양호Good 비교예1Comparative Example 1 층분리Layer separation 침전 후 cakingCaking after precipitation 층분리 후 cakingCaking after layer separation 층분리Layer separation 비교예2Comparative Example 2 층분리Layer separation 침전 후 cakingCaking after precipitation 층분리 후 cakingCaking after layer separation 층분리Layer separation 비교예3Comparative Example 3 층분리Layer separation 침전 후 cakingCaking after precipitation 층분리 후 cakingCaking after layer separation 층분리Layer separation

본 발명의 질화알미늄 분산액은 폴리아믹산을 분산제로 채용하여 제조함으로 플렉서블 기판에 사용되는 폴리이미드 필름의 방열성을 부여하는 것이 가능하게 되었다.The aluminum nitride dispersion of the present invention can be produced by employing polyamic acid as a dispersant, thereby making it possible to impart heat dissipation properties of a polyimide film used for a flexible substrate.

Claims (4)

10중량% 내지 50중량%의 질화붕소
1.0% 내지 10중량%의 폴리아믹산
30중량% 내지 80중량% 용매를 포함하는 방열용 분산액 조성물
10% to 50% by weight of boron nitride
1.0% to 10% by weight of polyamic acid
30% by weight to 80% by weight of a solvent;
제1항에 있어서, 평균입자경이 1내지 200㎚인 질화붕소가 10중량% 내지 50중량%로 포함되는 방열용 질화알미늄 분산액 조성물.The heat dissipation-use aluminum nitride dispersion composition according to claim 1, wherein 10 wt% to 50 wt% of boron nitride having an average particle size of 1 to 200 nm is contained. 제1항에 있어서, 폴리아믹산을 포함하는 방열용 질화붕소 분산액 조성물.The heat-dissipating boron nitride dispersion composition according to claim 1, comprising a polyamic acid. 제1항에 있어서,용매는 N-메틸피롤리돈(N-methylpyrrolidone), 디메틸아세트아미드(dimethylacetamide), 디아민(diamine), 디안하이드라이드(dianhydride), 디메틸포름아미드(dimethylformamide), 디메틸술폭시드 (dimethyl sulfoxide)로 이루어진 군에서 선택되는 1종 또는 2종 이상의 혼합물인 방열용 질화붕소 분산액 조성물.
The method of claim 1, wherein the solvent is selected from the group consisting of N-methylpyrrolidone, dimethylacetamide, diamine, dianhydride, dimethylformamide, dimethylsulfoxide dimethyl sulfoxide) or a mixture of two or more selected from the group consisting of boron nitride and boron nitride.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102017129472A1 (en) 2016-12-13 2018-06-14 Hyundai Motor Company Method and apparatus for heating a lambda sensor of a mild hybrid electric vehicle

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102017129472A1 (en) 2016-12-13 2018-06-14 Hyundai Motor Company Method and apparatus for heating a lambda sensor of a mild hybrid electric vehicle

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