KR20210036438A - A room-temperature fast curing conductive adhesive - Google Patents
A room-temperature fast curing conductive adhesive Download PDFInfo
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- KR20210036438A KR20210036438A KR1020190118053A KR20190118053A KR20210036438A KR 20210036438 A KR20210036438 A KR 20210036438A KR 1020190118053 A KR1020190118053 A KR 1020190118053A KR 20190118053 A KR20190118053 A KR 20190118053A KR 20210036438 A KR20210036438 A KR 20210036438A
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- room temperature
- epoxy resin
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- 239000000853 adhesive Substances 0.000 title claims abstract description 46
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 46
- 239000003822 epoxy resin Substances 0.000 claims abstract description 29
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 29
- -1 triphenyl ester Chemical class 0.000 claims abstract description 29
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 12
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 11
- 239000005011 phenolic resin Substances 0.000 claims abstract description 11
- 150000002989 phenols Chemical class 0.000 claims abstract description 11
- 229920000570 polyether Polymers 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 6
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 description 19
- 238000001879 gelation Methods 0.000 description 10
- 238000001556 precipitation Methods 0.000 description 9
- 230000032798 delamination Effects 0.000 description 7
- 239000012298 atmosphere Substances 0.000 description 6
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 description 6
- 238000001291 vacuum drying Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 229910001873 dinitrogen Inorganic materials 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 229910000679 solder Inorganic materials 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
- C09J163/10—Epoxy resins modified by unsaturated 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
- C08K3/02—Elements
- C08K3/08—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
- C08K3/34—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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/06—Ethers; Acetals; Ketals; Ortho-esters
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
-
- 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
- C08K2003/085—Copper
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/312—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier parameters being the characterizing feature
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Conductive Materials (AREA)
Abstract
Description
본 발명은 전자 재료 분야에 속하는 상온 속경화성 전도성 접착제, 및 이의 제조 방법 및 적용 방법에 관한 것이다.The present invention relates to a room temperature fast-curing conductive adhesive belonging to the field of electronic materials, and a method of manufacturing and applying the same.
전자 부품 및 구성요소들이 작아지고 가벼워짐에 따라, 마이크로 전자 패키징(microelectronic packaging) 산업에서 사용되는 기존의 Sn/Pb 솔더(solder)는 공정 요건을 충족시킬 수 없게 되었다. 따라서, 새로운 재료로서 전도성 접착제가 솔더 대신 전자 제품에 널리 사용되어왔다. 전도성 접착제는 경화 및 건조 후 특정 전도성 성능을 갖는 특수 접착제이다. 전도성 접착제는 경화제, 전도성 충전제(filler) 및 다른 첨가제들을 유기 고분자 매트릭스 수지에 첨가하여 제조된다. 전도성 접착제는 경화 후, 금속과 유사한 전도성 성능을 가지며, 동일한 유형 또는 상이한 유형의 전도성 물질들을 연결하여 연결된 물질들 사이에 전도성 루프를 형성할 수 있다. 따라서, 전도성 접착제는 Sn/Pb 솔더를 대체할 우수한 재료로 여겨진다. 구리 분말을 포함하는 전도성 접착제는 은 분말을 포함하는 전도성 접착제와 매우 유사한 전도성 성능을 가지며, 상대적으로 우수한 접합 강도 및 낮은 생산 비용을 가지므로 큰 주목을 받고 있다. 그러나, 현재의 전도성 접착제는 일반적으로 경화 시간이 너무 길다는 문제가 있어, 한편으로는 무전해 도금 제품의 코팅과 같이 몇 분 또는 수십 분 내에 완전히 경화되는 빠른 경화를 필요로 하는 많은 적용예에서의 요구 사항을 충족시키기 어렵고, 또한 경화 시간이 길면 생산 주기를 증가시켜 생산에 불리하다.As electronic components and components become smaller and lighter, conventional Sn/Pb solders used in the microelectronic packaging industry have become unable to meet process requirements. Therefore, as a new material, conductive adhesives have been widely used in electronic products instead of solder. Conductive adhesives are special adhesives that have specific conductive properties after curing and drying. Conductive adhesives are prepared by adding a curing agent, a conductive filler, and other additives to an organic polymer matrix resin. After curing, the conductive adhesive has a conductive performance similar to that of a metal, and can connect conductive materials of the same type or different types to form a conductive loop between the connected materials. Therefore, conductive adhesives are considered to be excellent materials to replace Sn/Pb solders. The conductive adhesive containing copper powder has a conductive performance very similar to that of the conductive adhesive containing silver powder, and is attracting great attention because it has relatively excellent bonding strength and low production cost. However, current conductive adhesives generally have a problem that the curing time is too long, on the one hand, in many applications requiring fast curing that completely cures within minutes or tens of minutes, such as coatings of electroless plated products. It is difficult to meet the requirements, and if the curing time is long, the production cycle is increased, which is disadvantageous to production.
종래 기술에 존재하는 상술한 문제점을 해결하기 위해, 본 발명은 상온에서 빠르게 경화될 수 있는 트리페닐 에스테르 에폭시 수지 전도성 접착제, 및 이의 제조 방법 및 적용 방법을 제공한다.In order to solve the above-described problems present in the prior art, the present invention provides a triphenyl ester epoxy resin conductive adhesive that can be rapidly cured at room temperature, and a method of manufacturing and applying the same.
본 발명의 트리페닐 에스테르 에폭시 수지 전도성 접착제는The triphenyl ester epoxy resin conductive adhesive of the present invention
트리페닐 에스테르 에폭시 수지 100 중량부,100 parts by weight of triphenyl ester epoxy resin,
부틸화 페놀 수지 50 내지 150 중량부,50 to 150 parts by weight of a butylated phenol resin,
폴리에테르 2 내지 10 중량부,2 to 10 parts by weight of polyether,
트리페닐 에스테르 에폭시 수지 경화제 50 내지 90 중량부,Triphenyl ester epoxy resin curing agent 50 to 90 parts by weight,
경화 촉진제 3 내지 6 중량부,3 to 6 parts by weight of a curing accelerator,
구리 분말 200 내지 1600 중량부, 및200 to 1600 parts by weight of copper powder, and
나노-실리카 2 내지 4 중량부로 주로 구성된다.It is mainly composed of 2 to 4 parts by weight of nano-silica.
본 발명의 트리페닐 에스테르 에폭시 수지 전도성 접착제는 하기 단계들을 포함하는 방법에 의해 제조될 수 있다:The triphenyl ester epoxy resin conductive adhesive of the present invention can be prepared by a method comprising the following steps:
(1) 구리 분말의 칭량하고, 상기 구리 분말의 총 중량을 기준으로 1 내지 3%의 실란 커플링제를 첨가하여 혼합물을 얻고, 적절한 양의 유기 용매를 상기 혼합물에 첨가하고, 결과물을 초음파 분쇄기로 30 내지 40분간 초음파 변형하고, 변형된 결과물을 증발 접시에 붓고 진공 건조하는 단계; 및(1) Weighing the copper powder and adding 1 to 3% of a silane coupling agent based on the total weight of the copper powder to obtain a mixture, an appropriate amount of an organic solvent was added to the mixture, and the resultant was subjected to an ultrasonic grinder. Ultrasonically transforming for 30 to 40 minutes, pouring the transformed product into an evaporation dish, and vacuum drying; And
(2) 상기 단계 (1)에서 제조된 결과물에 트리페닐 에스테르 에폭시 수지, 트리페닐 에스테르 에폭시 수지 경화제, 경화 촉진제, 부틸화 페놀 수지, 폴리에테르 및 나노-실리카를 상온에서 첨가하여 혼합물을 얻고, 상기 혼합물을 30 내지 40분간 진공 교반하여 트리페닐 에스테르 에폭시 수지 전도성 접착제를 얻는 단계.(2) Triphenyl ester epoxy resin, triphenyl ester epoxy resin curing agent, curing accelerator, butylated phenol resin, polyether and nano-silica were added to the resultant product prepared in step (1) at room temperature to obtain a mixture, and the Vacuum stirring the mixture for 30 to 40 minutes to obtain a triphenyl ester epoxy resin conductive adhesive.
또한, 본 발명은 대기 환경에서 상기 전도성 접착제를 기판의 표면에 도포하고, 상기 전도성 접착제를 상온에서 경화시키는 단계를 포함하는, 트리페닐 에스테르 에폭시 수지 전도성 접착제의 적용 방법을 제공한다.In addition, the present invention provides a method of applying a triphenyl ester epoxy resin conductive adhesive comprising the step of applying the conductive adhesive to the surface of a substrate in an atmospheric environment and curing the conductive adhesive at room temperature.
종래 기술의 전도성 접착제와 비교하여, 본 발명은 다음과 같은 장점 및 유리한 효과를 갖는다.Compared with the conductive adhesive of the prior art, the present invention has the following advantages and advantageous effects.
(1) 대기 분위기의 상온에서 부틸화 페놀 수지 및 폴리에테르의 발열 중합에 의해, 본 발명의 전도성 접착제는 20분 미만의 경화 시간 내에, 추가적인 가열 없이 상온에서 속경화를 구현한다. 본 발명의 전도성 접착제는 14MPa보다 높은 전단 강도를 가지며, 우수한 내열성, 내후성 및 내습성을 가지며, 겔화(gelation)없이 상온에서 2개월 이상 보관할 수 있다.(1) By exothermic polymerization of butylated phenol resin and polyether at room temperature in an atmospheric atmosphere, the conductive adhesive of the present invention realizes fast curing at room temperature without additional heating within a curing time of less than 20 minutes. The conductive adhesive of the present invention has a shear strength higher than 14 MPa, has excellent heat resistance, weather resistance, and moisture resistance, and can be stored for 2 months or more at room temperature without gelation.
(2) 상기 전도성 접착제에 특정 비율의 나노-실리카를 첨가함으로써, 본 발명의 전도성 접착제는 속경화 구현과 함께, 현저한 강화 및 강인화 효과를 달성하고 30% 개선된 결합 강도를 제공한다.(2) By adding a specific ratio of nano-silica to the conductive adhesive, the conductive adhesive of the present invention achieves remarkable strengthening and toughening effects with fast curing, and provides 30% improved bonding strength.
(3) 구리 분말을 표면 처리하고 그 양을 본 발명에 설명된 범위 내로 제어함으로써, 수득된 전도성 접착제는 2 x 10-6Ω·m 미만의 체적 저항률을 갖는다.(3) By surface-treating the copper powder and controlling its amount within the range described in the present invention, the obtained conductive adhesive has a volume resistivity of less than 2 x 10 -6 Ω·m.
본 발명은 이하의 예시적인 실시예들에 의해 추가로 설명되지만, 본 발명은 아래에 기재된 특정 실시예들에 제한되지 않는다.The invention is further illustrated by the following exemplary embodiments, but the invention is not limited to the specific embodiments described below.
실시예 1Example 1
500 중량부의 구리 분말을 칭량하고, 거기에 무수 에탄올에 용해된 10 중량부의 KH550을 첨가하고, 수득된 혼합물을 30분 동안 초음파로 교반한 다음, 진공 건조기에서 건조시키고 밀봉하였다.500 parts by weight of copper powder was weighed, 10 parts by weight of KH550 dissolved in absolute ethanol was added thereto, and the obtained mixture was stirred ultrasonically for 30 minutes, then dried in a vacuum dryer and sealed.
구리 분말을 포함하는 위에서 얻어진 결과물에 트리페닐 에스테르 에폭시 수지 100 중량부, 부틸화 페놀 수지 100 중량부, 폴리에테르 5 중량부, 메틸헥사히드로프탈산 무수물 60 중량부, MY-24 5 중량부 및 나노-실리카 3 중량부를 상온의 질소 가스 분위기 하에서 순차적으로 첨가하여 혼합물을 얻었다. 그리고 상기 혼합물을 균일하게 혼합하고 진공 건조 오븐에 넣어 기포를 제거하여 트리페닐 에스테르 에폭시 수지 전도성 접착제 A를 얻었다.To the result obtained above containing copper powder, 100 parts by weight of triphenyl ester epoxy resin, 100 parts by weight of butylated phenol resin, 5 parts by weight of polyether, 60 parts by weight of methylhexahydrophthalic anhydride, 5 parts by weight of MY-24 and nano- 3 parts by weight of silica was sequentially added under a nitrogen gas atmosphere at room temperature to obtain a mixture. Then, the mixture was uniformly mixed and placed in a vacuum drying oven to remove air bubbles to obtain a triphenyl ester epoxy resin conductive adhesive A.
실시예 2Example 2
1500 중량부의 구리 분말의 무게를 달고, 거기에 무수 에탄올에 용해된 25 중량부의 KH550을 첨가하고, 수득된 혼합물질을 30분 동안 초음파로 교반한 다음, 진공 건조기에서 건조시키고 밀봉하였다.1500 parts by weight of copper powder was weighed, 25 parts by weight of KH550 dissolved in absolute ethanol was added thereto, and the obtained mixture was stirred ultrasonically for 30 minutes, then dried in a vacuum dryer and sealed.
구리 분말을 포함하는 위에서 얻어진 결과물에 트리페닐 에스테르 에폭시 수지 100 중량부, 부틸화 페놀 수지 130 중량부, 폴리에테르 7 중량부, 메틸헥사히드로프탈산 무수물 75 중량부, MY-24 4 중량부 및 나노-실리카 2.5 중량부를 상온의 질소 가스 분위기 하에서 순차적으로 첨가하여 혼합물을 얻었다. 그리고 상기 혼합물을 균일하게 혼합하고 진공 건조 오븐에 넣어 기포를 제거하여 트리페닐 에스테르 에폭시 수지 전도성 접착제 B를 얻었다.To the result obtained above containing copper powder, 100 parts by weight of triphenyl ester epoxy resin, 130 parts by weight of butylated phenol resin, 7 parts by weight of polyether, 75 parts by weight of methylhexahydrophthalic anhydride, 4 parts by weight of MY-24 and nano- 2.5 parts by weight of silica was sequentially added under a nitrogen gas atmosphere at room temperature to obtain a mixture. Then, the mixture was uniformly mixed and placed in a vacuum drying oven to remove air bubbles to obtain a triphenyl ester epoxy resin conductive adhesive B.
실시예 3Example 3
1300 중량부의 구리 분말의 무게를 달고, 거기에 무수 에탄올에 용해된 17 중량부의 KH550을 첨가하고, 수득된 혼합물질을 30분 동안 초음파로 교반한 다음, 진공 건조기에서 건조시키고 밀봉하였다.1300 parts by weight of copper powder was weighed, 17 parts by weight of KH550 dissolved in absolute ethanol was added thereto, and the obtained mixture was stirred ultrasonically for 30 minutes, then dried in a vacuum dryer and sealed.
구리 분말을 포함하는 위에서 얻어진 결과물에 트리페닐 에스테르 에폭시 수지 100 중량부, 부틸화 페놀 수지 125 중량부, 폴리에테르 7.5 중량부, 메틸헥사히드로프탈산 무수물 80 중량부, MY-24 3 중량부 및 나노-실리카 3.5 중량부를 상온의 질소 가스 분위기 하에서 순차적으로 첨가하여 혼합물을 얻었다. 그리고 상기 혼합물을 균일하게 혼합하고 진공 건조 오븐에 넣어 기포를 제거하여 트리페닐 에스테르 에폭시 수지 전도성 접착제 C를 얻었다.To the result obtained above containing copper powder, 100 parts by weight of triphenyl ester epoxy resin, 125 parts by weight of butylated phenol resin, 7.5 parts by weight of polyether, 80 parts by weight of methylhexahydrophthalic anhydride, 3 parts by weight of MY-24 and nano- 3.5 parts by weight of silica was sequentially added under a nitrogen gas atmosphere at room temperature to obtain a mixture. Then, the mixture was uniformly mixed and placed in a vacuum drying oven to remove air bubbles to obtain a triphenyl ester epoxy resin conductive adhesive C.
실시예 4Example 4
800 중량부의 구리 분말의 무게를 달고, 거기에 무수 에탄올에 용해된 8 중량부의 KH550을 첨가하고, 수득된 혼합물질을 30분 동안 초음파로 교반한 다음, 진공 건조기에서 건조시키고 밀봉하였다.800 parts by weight of copper powder was weighed, and 8 parts by weight of KH550 dissolved in absolute ethanol was added thereto, and the obtained mixture was stirred ultrasonically for 30 minutes, then dried in a vacuum dryer and sealed.
구리 분말을 포함하는 위에서 얻어진 결과물에 트리페닐 에스테르 에폭시 수지 100 중량부, 부틸화 페놀 수지 90 중량부, 폴리에테르 3.5 중량부, 메틸헥사히드로프탈산 무수물 70 중량부, MY-24 4 중량부 및 나노-실리카 2 중량부를 상온의 질소 가스 분위기 하에서 순차적으로 첨가하여 혼합물을 얻었다. 그리고 상기 혼합물을 균일하게 혼합하고 진공 건조 오븐에 넣어 기포를 제거하여 트리페닐 에스테르 에폭시 수지 전도성 접착제 D를 얻었다.To the result obtained above containing copper powder, 100 parts by weight of triphenyl ester epoxy resin, 90 parts by weight of butylated phenol resin, 3.5 parts by weight of polyether, 70 parts by weight of methylhexahydrophthalic anhydride, 4 parts by weight of MY-24 and nano- 2 parts by weight of silica were sequentially added under a nitrogen gas atmosphere at room temperature to obtain a mixture. Then, the mixture was uniformly mixed and placed in a vacuum drying oven to remove air bubbles to obtain a triphenyl ester epoxy resin conductive adhesive D.
실시예 5Example 5
1000 중량부의 구리 분말의 무게를 달고, 거기에 무수 에탄올에 용해된 20 중량부의 KH550을 첨가하고, 수득된 혼합물질을 30분 동안 초음파로 교반한 다음, 진공 건조기에서 건조시키고 밀봉하였다.1000 parts by weight of copper powder was weighed, 20 parts by weight of KH550 dissolved in absolute ethanol was added thereto, and the obtained mixture was stirred ultrasonically for 30 minutes, then dried in a vacuum dryer and sealed.
구리 분말을 포함하는 위에서 얻어진 결과물에 트리페닐 에스테르 에폭시 수지 100 중량부, 부틸화 페놀 수지 140 중량부, 폴리에테르 9 중량부, 메틸헥사히드로프탈산 무수물 90 중량부, MY-24 6 중량부 및 나노-실리카 3 중량부를 상온의 질소 가스 분위기 하에서 순차적으로 첨가하여 혼합물을 얻었다. 그리고 상기 혼합물을 균일하게 혼합하고 진공 건조 오븐에 넣어 기포를 제거하여 트리페닐 에스테르 에폭시 수지 전도성 접착제 E를 얻었다.To the result obtained above containing copper powder, 100 parts by weight of triphenyl ester epoxy resin, 140 parts by weight of butylated phenol resin, 9 parts by weight of polyether, 90 parts by weight of methylhexahydrophthalic anhydride, 6 parts by weight of MY-24 and nano- 3 parts by weight of silica was sequentially added under a nitrogen gas atmosphere at room temperature to obtain a mixture. Then, the mixture was uniformly mixed and placed in a vacuum drying oven to remove air bubbles to obtain a triphenyl ester epoxy resin conductive adhesive E.
비교예 1Comparative Example 1
메틸헥사히드로프탈산 무수물 및 경화 촉진제 MY-24 대신에 저분자 폴리아미드를 사용하고, 부틸화 페놀 수지 및 폴리 에테르를 사용하지 않은 것을 제외하고는, 실시예 1과 동일한 방법으로 트리페닐 에스테르 에폭시 수지 전도성 접착제 X를 제조 하였다.Triphenyl ester epoxy resin conductive adhesive in the same manner as in Example 1, except that a low molecular weight polyamide was used instead of the methylhexahydrophthalic anhydride and the curing accelerator MY-24, and a butylated phenol resin and a polyether were not used. X was prepared.
비교예 2Comparative Example 2
나노-실리카를 사용하지 않은 것을 제외하고는 실시예 1과 동일한 방법으로 트리페닐 에스테르 에폭시 수지 전도성 접착제 Y를 제조 하였다.A triphenyl ester epoxy resin conductive adhesive Y was prepared in the same manner as in Example 1, except that nano-silica was not used.
비교예 3Comparative Example 3
나노-실리카 5 중량부를 사용한 것을 제외하고는 실시예 1과 동일한 방법으로 트리페닐 에스테르 에폭시 수지 전도성 접착제 Z를 제조 하였다.A triphenyl ester epoxy resin conductive adhesive Z was prepared in the same manner as in Example 1, except that 5 parts by weight of nano-silica was used.
시험 방법Test Methods
(1) 체적 저항률: GB/T 1410-2006에 따라 시험하였다.(1) Volume resistivity: It was tested according to GB/T 1410-2006.
(2) 전단 강도: GB/T 7124-2008에 따라, 접합된 철판을 공기 중에 놓아 시험용으로 상온에서 20분간 경화시켰다.(2) Shear strength: According to GB/T 7124-2008, the bonded steel plate was placed in air and cured at room temperature for 20 minutes for testing.
(3) 저장 안정성: 얻어진 전도성 접착제를 5mL 투명 주사기에 넣고 상온에서 2개월 동안 보관한 후 겔화, 박리 또는 침전에 대해 육안으로 검사하였다.(3) Storage stability: The obtained conductive adhesive was placed in a 5 mL transparent syringe and stored at room temperature for 2 months, and then visually inspected for gelation, peeling, or precipitation.
(4) 경화 시간: 트리페닐 에스테르 에폭시 수지 전도성 접착제가 안정한 체적 저항률 및 안정한 접착 강도를 얻기 위해 필요한 시간이다.(4) Curing time: This is the time required for the triphenyl ester epoxy resin conductive adhesive to obtain a stable volume resistivity and stable adhesive strength.
결과는 아래 표 1에 나타내었다.The results are shown in Table 1 below.
(Ω·m) Volume resistivity
(Ω·m)
(MPa)Shear strength
(MPa)
(25℃，2개월)Storage stability
(25℃, 2 months)
표 1에서 알 수 있듯이, 본 발명의 경화 시스템을 채택한 전도성 접착제는 상온에서 15분 이내에 빠르게 경화될 수 있으며, 본 발명의 경화 시스템을 채택하지 않은 전도성 접착제와 비교하여 개선된 전단 강도 및 개선된 저장 안정성을 가진다. 또한, 전도성 접착제 X-Z와 비교하여, 본 발명의 모든 전도성 접착제들은 열화 없이 실질적으로 동일한 수준으로 유지된 체적 저항률을 가진다.As can be seen from Table 1, the conductive adhesive adopting the curing system of the present invention can be rapidly cured within 15 minutes at room temperature, and has improved shear strength and improved storage compared to the conductive adhesive without the curing system of the present invention. Have stability. Further, compared to the conductive adhesive X-Z, all the conductive adhesives of the present invention have a volume resistivity maintained at substantially the same level without deterioration.
상술한 것은 오직 본 발명의 실시예들에 대한 설명이며, 공지의 구체적인 구성 및 특징에 대해서는 설명하지 않았다. 유의해야 할 점은, 본 발명의 사상을 벗어나지 않고 당업자에 의해 많은 변형 및 수정이 이루어질 수 있으며, 이러한 모든 변형 및 수정은 본 발명의 보호 범위로 간주되어야 하며, 그것들은 본 발명의 구현 효과 및 그 특허 실행에 영향을 미치지 않을 것이다. 본 출원에 의해 청구된 보호 범위는 청구 범위의 내용에 기초해야 하고, 명세서에 인용된 특정 실시예 등이 청구 범위의 내용을 설명하는데 사용될 수 있다.What has been described above is only a description of embodiments of the present invention, and well-known specific configurations and features are not described. It should be noted that many variations and modifications may be made by those skilled in the art without departing from the spirit of the present invention, and all such modifications and modifications should be considered as the scope of protection of the present invention, and they are It will not affect the execution of the patent. The scope of protection claimed by this application should be based on the content of the claims, and specific embodiments and the like cited in the specification may be used to describe the content of the claims.
Claims (5)
부틸화 페놀 수지 50 내지 150 중량부,
폴리에테르 2 내지 10 중량부,
트리페닐 에스테르 에폭시 수지 경화제 50 내지 90 중량부,
경화 촉진제 3 내지 6 중량부,
구리 분말 200 내지 1600 중량부, 및
나노-실리카 2 내지 4 중량부를 포함하며,
상기 구리 분말은 실란 커플링제에 의해 표면 개질되고, 상온에서 20분 이내에 경화되는, 상온 속경화성 전도성 접착제.100 parts by weight of triphenyl ester epoxy resin,
50 to 150 parts by weight of a butylated phenol resin,
2 to 10 parts by weight of polyether,
Triphenyl ester epoxy resin curing agent 50 to 90 parts by weight,
3 to 6 parts by weight of a curing accelerator,
200 to 1600 parts by weight of copper powder, and
It contains 2 to 4 parts by weight of nano-silica,
The copper powder is surface-modified by a silane coupling agent and cured at room temperature within 20 minutes.
The room temperature fast-curing conductive adhesive according to claim 1, having a volume resistivity of less than 2Х10 -6 Ω·m.
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