KR20210030099A - A room-temperature fast curing conductive adhesive - Google Patents
A room-temperature fast curing conductive adhesive Download PDFInfo
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- KR20210030099A KR20210030099A KR1020190111629A KR20190111629A KR20210030099A KR 20210030099 A KR20210030099 A KR 20210030099A KR 1020190111629 A KR1020190111629 A KR 1020190111629A KR 20190111629 A KR20190111629 A KR 20190111629A KR 20210030099 A KR20210030099 A KR 20210030099A
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- conductive adhesive
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- epoxy resin
- dimethyl ester
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- 239000000853 adhesive Substances 0.000 title claims abstract description 50
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 50
- 239000003822 epoxy resin Substances 0.000 claims abstract description 29
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 29
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 12
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 11
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 11
- 125000002496 methyl group Chemical group [H]C([H])([H])* 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
- 238000001879 gelation Methods 0.000 claims description 11
- 238000001556 precipitation Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 7
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 description 19
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 description 6
- 238000003756 stirring Methods 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
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 229910000679 solder Inorganic materials 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005303 weighing Methods 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
- 239000000654 additive Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- QUQFTIVBFKLPCL-UHFFFAOYSA-L copper;2-amino-3-[(2-amino-2-carboxylatoethyl)disulfanyl]propanoate Chemical compound [Cu+2].[O-]C(=O)C(N)CSSCC(N)C([O-])=O QUQFTIVBFKLPCL-UHFFFAOYSA-L 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000011156 evaluation Methods 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
- 229910052742 iron Inorganic materials 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
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 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
- 230000008569 process Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000000758 substrate Substances 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
-
- 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
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
-
- 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
- C08L61/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08L61/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08L61/28—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with melamine
-
- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. 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
- 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
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
-
- 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 실온 속경화형 도전성 접착제, 그 준비 방법 및 전자 재료 분야로의 응용 방법에 관한 것이다.The present invention relates to a room temperature fast curing type conductive adhesive, a preparation method thereof, and an application method to the field of electronic materials.
전자 부품 및 구성 요소들이 작아지고 가벼워짐에 따라, 마이크로일렉트로닉 패키징 산업에서 사용되는 종래의 주석/납(Sn/Pb) 솔더는 공정 요건을 만족하지 못하게 되었다. 따라서, 새로운 물질로서, 도전성 접착제가 솔더를 대신하여 전자 제품에 널리 사용되고 있다. 상기 도전성 접착제는 경화/건조 후에 특정한 도전 성능을 갖는 특별한 접착제이다. 상기 도전성 접착제는 경화제, 도전성 필러 및 다른 첨가제들을 유기 고분자 매트릭스 수지에 혼합하여 준비된다. 상기 도전성 접착제는 경화된 후에 금속에 가까운 도전 성능을 가지며, 동일한 타입 또는 다른 타입의 도전성 물질들을 연결함으로써 연결되는 물질들 사이에 도전성 루프를 형성할 수 있다. 따라서, 상기 도전성 접착제는 주석/납 솔더를 대신하는 훌륭한 물질로 간주된다. 구리 파우더를 포함하는 도전성 물질은, 은 파우더를 포함하는 도전성 접착제에 매우 가까운 도전 성능을 가지며, 상대적으로 우수한 결합력과 낮은 단가로 인하여 많은 관심을 끌고 있다. 그러나, 현재의 도전성 접착제는 경화 시간이 너무 긴 문제가 있다. 이에 따라, 무전해 도금 제품과 같이, 수분에서 10분 사이에 도전성 접착제가 완전히 경화되어야 하는 속경화를 요구하는 많은 응용 분야의 요구를 충족하기 어려울 뿐만 아니라, 긴 경화 시간은 긴 생산 사이클로 이어져, 생산에 유리하지 않다.As electronic components and components become smaller and lighter, conventional tin/lead (Sn/Pb) solders used in the microelectronic packaging industry have failed to meet process requirements. Therefore, as a new material, conductive adhesives are widely used in electronic products in place of solder. The conductive adhesive is a special adhesive having a specific conductive performance after curing/drying. The conductive adhesive is prepared by mixing a curing agent, a conductive filler, and other additives with an organic polymer matrix resin. The conductive adhesive has a conductive performance close to that of a metal after being cured, and may form a conductive loop between the connected materials by connecting conductive materials of the same type or different types. Therefore, the conductive adhesive is considered an excellent substitute for tin/lead solder. A conductive material containing copper powder has a conductive performance very close to that of a conductive adhesive containing silver powder, and is attracting a lot of attention due to relatively excellent bonding strength and low cost. However, the current conductive adhesive has a problem that the curing time is too long. Accordingly, it is difficult to meet the demands of many applications that require fast curing in which the conductive adhesive must be completely cured within 10 minutes, such as electroless plating products, and the long curing time leads to a long production cycle, resulting in production. Not in favor of
본 발명의 목적은 종래 기술에 존재하는 위와 같은 문제점들을 해결하기 위한 것으로서, 본 발명은, 실온에서 빠르게 경화될 수 있는 O-디메틸 에스터 에폭시 수지 도전성 접착제, 그 준비 방법 및 응용 방법을 제공한다.An object of the present invention is to solve the above problems existing in the prior art, and the present invention provides an O-dimethyl ester epoxy resin conductive adhesive that can be rapidly cured at room temperature, a preparation method and an application method thereof.
본 발명에 따른 O-디메틸 에스터 에폭시 수지 도전성 접착제는,O-dimethyl ester epoxy resin conductive adhesive according to the present invention,
O-디메틸 에스터 에폭시 수지 100 중량부, 100 parts by weight of O-dimethyl ester epoxy resin,
로우(low) 메틸 에테르화 멜라민 포름알데하이드 수지 50-150 중량부,50-150 parts by weight of low methyl etherified melamine formaldehyde resin,
폴리에테르 2-10 중량부,2-10 parts by weight of polyether,
O-디메틸 에스터 에폭시 수지 경화제 50-90 중량부,O-dimethyl ester epoxy resin curing agent 50-90 parts by weight,
경화 촉진제 3-6 중량부,3-6 parts by weight of a hardening accelerator,
구리 파우더 200-1600 중량부 및200-1600 parts by weight of copper powder and
나노 실리카 2-4 중량부로 주로 이루어진다.It mainly consists of 2-4 parts by weight of nano silica.
본 발명에 따른 O-디메틸 에스터 에폭시 수지 도전성 접착제의 준비 방법은, (1) 구리 파우더를 칙량하고(weighing), 구리 파우더 전체 중량에 대하여 1%-3%의 실란 커플링제를 더하여 혼합물을 얻고, 상기 혼합물에 적절한 양의 유기 용매를 더하고, 그 결과물을, 30-40분간 초음파 미분쇄기(pulverizer)로 초음파 개질하고, 상기 개질된 결과물을 증발 접시에 붓고, 그리고 진공 건조를 수행하는 단계; 및The preparation method of the O-dimethyl ester epoxy resin conductive adhesive according to the present invention includes (1) weighing copper powder, and adding 1%-3% of a silane coupling agent to the total weight of the copper powder to obtain a mixture, Adding an appropriate amount of an organic solvent to the mixture, ultrasonically modifying the resultant product with an ultrasonic pulverizer for 30-40 minutes, pouring the modified product into an evaporation dish, and performing vacuum drying; And
(2) 실온에서, O-디메틸 에스터 에폭시 수지, O-디메틸 에스터 에폭시 수지 경화제, 경화 촉진제, 로우 메틸 에테르화 멜라민 포름알데하이드 수지, 폴리에테르 및 나노 실리카를 단계(1)에서 준비된 결과물에 더하여 혼합물을 얻고, 30-40분간 상기 혼합물을 진공 교반하여 O-디메틸 에스터 에폭시 수지 도전성 접착제를 얻는 단계를 포함한다.(2) At room temperature, O-dimethyl ester epoxy resin, O-dimethyl ester epoxy resin curing agent, curing accelerator, low methyl etherified melamine formaldehyde resin, polyether and nano silica were added to the resultant prepared in step (1) to prepare a mixture. And vacuum stirring the mixture for 30-40 minutes to obtain an O-dimethyl ester epoxy resin conductive adhesive.
또한, 본 발명은, 상기 도전성 접착제를 대기 환경에서 기재(substrate)의 표면에 제공하는 단계, 및 상기 도전성 접착제를 실온에서 경화하는 단계를 포함하는, 상기 O-디메틸 에스터 에폭시 수지 도전성 접착제의 응용 방법을 제공한다.In addition, the present invention, comprising the step of providing the conductive adhesive on the surface of a substrate in an atmospheric environment, and curing the conductive adhesive at room temperature, the application method of the O-dimethyl ester epoxy resin conductive adhesive Provides.
종래의 도전성 접착제와 비교하여, 본 발명은 다음의 이점과 유리한 효과들을 갖는다.Compared with the conventional conductive adhesive, the present invention has the following advantages and advantageous effects.
(1) 실온 및 대기 환경에서 로우 메틸 에테르화 멜라민 포름알데하이드 수지와 폴리에테르의 발열성 중합에 의해, 본 발명의 도전성 접착제는 추가적인 가열 없이 실온에서 20분 미만의 경화 시간으로 속경화를 달성할 수 있다. 본 발명의 도전성 접착제는 14MPa 보다 높은 전단 강도(shear strength)를 가지며, 우수한 내열성, 내후성 및 내습성을 갖는다. 또한, 겔화 없이 2개월 이상 실온에서 보관될 수 있다.(1) By exothermic polymerization of low methyl etherified melamine formaldehyde resin and polyether in room temperature and atmospheric environment, the conductive adhesive of the present invention can achieve fast curing with less than 20 minutes curing time at room temperature without additional heating. have. The conductive adhesive of the present invention has a shear strength higher than 14 MPa, and has excellent heat resistance, weather resistance, and moisture resistance. In addition, it can be stored at room temperature for at least 2 months without gelation.
(2) 상기 도전성 접착제에 나노 실리카를 특정한 비율로 더함으로써, 본 발명의 도전성 접착제는, 현저한 보강 및 강인화(strengthening and toughening) 효과를 달성하고, 결합 강도를 30%까지 개선하면서 속경화를 달성할 수 있다. (2) By adding nano silica in a specific ratio to the conductive adhesive, the conductive adhesive of the present invention achieves remarkable reinforcing and toughening effects, and achieves fast curing while improving the bonding strength up to 30%. can do.
(3) 상기 구리 파우더를 표면 처리하고, 그 함량을 본 발명에 개시된 함량 이내로 조절함으로써, 얻어진 도전성 접착제는 2×10- 6Ωㆍm 미만의 체적 저항률(volume resistivity)을 갖는다.(3) surface treating the copper powder, and, by adjusting the content within the content disclosed in the present invention, the obtained conductive adhesive is 2 × 10 - has an Ω less than 6 m and a volume resistivity of (volume resistivity).
본 발명은 다음의 실시예들에 의해 보다 구체적으로 설명되나, 본 발명은 아래에 기재된 특정 실시예들로 한정되는 것은 아니다.The present invention is described in more detail by the following examples, but the present invention is not limited to the specific examples described below.
실시예 1Example 1
구리 파우더 500 중량부를 무게를 달아, 무수 에탄올(absolute ethanol)에 용해된 KH550 10 중량부를 추가하였다. 얻어진 혼합물을 30분간 초음파 교반한 후, 진공 건조기에서 건조하고, 밀봉하였다.500 parts by weight of copper powder was weighed, and 10 parts by weight of KH550 dissolved in absolute ethanol was added. After ultrasonically stirring the obtained mixture for 30 minutes, it was dried in a vacuum dryer and sealed.
실온 및 질소 가스 환경에서, 상기에서 얻어진 구리 파우더를 함유하는 결과물에 O-디메틸 에스터 에폭시 수지 100 중량부, 로우 메틸 에테르화 멜라민 포름알데하이드 수지 100 중량부, 폴리에테르 5 중량부, 메틸헥사하이드로프탈릭 무수물(methylhexahydrophthalic anhydride) 60 중량부, MY-24 5 중량부 및 나노 실리카 3 중량부를 연속으로 더하여 혼합물을 얻었다. 상기 혼합물을 균일하게 혼합하고, 진공 건조 오븐에 두어 기포를 제거함으로써, O-디메틸 에스터 에폭시 수지 도전성 접착제 A를 얻었다.In a room temperature and nitrogen gas environment, in the resultant product containing the copper powder obtained above, 100 parts by weight of O-dimethyl ester epoxy resin, 100 parts by weight of low methyl etherified melamine formaldehyde resin, 5 parts by weight of polyether, methylhexahydrophthalic 60 parts by weight of methylhexahydrophthalic anhydride, 5 parts by weight of MY-24, and 3 parts by weight of nano silica were successively added to obtain a mixture. The mixture was uniformly mixed and placed in a vacuum drying oven to remove air bubbles, thereby obtaining an O-dimethyl ester epoxy resin conductive adhesive A.
실시예 2Example 2
구리 파우더 1500 중량부를 무게를 달아, 무수 에탄올에 용해된 KH550 25 중량부를 추가하였다. 얻어진 혼합물을 30분간 초음파 교반한 후, 진공 건조기에서 건조하고, 밀봉하였다.1500 parts by weight of copper powder was weighed, and 25 parts by weight of KH550 dissolved in absolute ethanol was added. After ultrasonically stirring the obtained mixture for 30 minutes, it was dried in a vacuum dryer and sealed.
실온 및 질소 가스 환경에서, 상기에서 얻어진 구리 파우더를 함유하는 결과물에 O-디메틸 에스터 에폭시 수지 100 중량부, 로우 메틸 에테르화 멜라민 포름알데하이드 수지 130 중량부, 폴리에테르 7 중량부, 메틸헥사하이드로프탈릭 무수물(methylhexahydrophthalic anhydride) 75 중량부, MY-24 4 중량부 및 나노 실리카 2.5 중량부를 연속으로 더하여 혼합물을 얻었다. 상기 혼합물을 균일하게 혼합하고, 진공 건조 오븐에 두어 기포를 제거함으로써, O-디메틸 에스터 에폭시 수지 도전성 접착제 B를 얻었다.In a room temperature and nitrogen gas environment, in the resultant product containing the copper powder obtained above, 100 parts by weight of O-dimethyl ester epoxy resin, 130 parts by weight of low methyl etherified melamine formaldehyde resin, 7 parts by weight of polyether, methylhexahydrophthalic 75 parts by weight of methylhexahydrophthalic anhydride, 4 parts by weight of MY-24, and 2.5 parts by weight of nano silica were successively added to obtain a mixture. The mixture was uniformly mixed and placed in a vacuum drying oven to remove air bubbles, thereby obtaining an O-dimethyl ester epoxy resin conductive adhesive B.
실시예 3Example 3
구리 파우더 1300 중량부를 무게를 달아, 무수 에탄올에 용해된 KH550 17 중량부를 추가하였다. 얻어진 혼합물을 30분간 초음파 교반한 후, 진공 건조기에서 건조하고, 밀봉하였다.1300 parts by weight of copper powder was weighed, and 17 parts by weight of KH550 dissolved in absolute ethanol was added. After ultrasonically stirring the obtained mixture for 30 minutes, it was dried in a vacuum dryer and sealed.
실온 및 질소 가스 환경에서, 상기에서 얻어진 구리 파우더를 함유하는 결과물에 O-디메틸 에스터 에폭시 수지 100 중량부, 로우 메틸 에테르화 멜라민 포름알데하이드 수지 125 중량부, 폴리에테르 7.5 중량부, 메틸헥사하이드로프탈릭 무수물(methylhexahydrophthalic anhydride) 80 중량부, MY-24 3 중량부 및 나노 실리카 3.5 중량부를 연속으로 더하여 혼합물을 얻었다. 상기 혼합물을 균일하게 혼합하고, 진공 건조 오븐에 두어 기포를 제거함으로써, O-디메틸 에스터 에폭시 수지 도전성 접착제 C를 얻었다.In a room temperature and nitrogen gas environment, in the resultant product containing the copper powder obtained above, 100 parts by weight of O-dimethyl ester epoxy resin, 125 parts by weight of low methyl etherified melamine formaldehyde resin, 7.5 parts by weight of polyether, methylhexahydrophthalic 80 parts by weight of methylhexahydrophthalic anhydride, 3 parts by weight of MY-24, and 3.5 parts by weight of nano silica were successively added to obtain a mixture. The mixture was uniformly mixed and placed in a vacuum drying oven to remove air bubbles, thereby obtaining an O-dimethyl ester epoxy resin conductive adhesive C.
실시예 4Example 4
구리 파우더 800 중량부를 무게를 달아, 무수 에탄올에 용해된 KH550 8 중량부를 추가하였다. 얻어진 혼합물을 30분간 초음파 교반한 후, 진공 건조기에서 건조하고, 밀봉하였다.After weighing 800 parts by weight of copper powder, 8 parts by weight of KH550 dissolved in absolute ethanol was added. After ultrasonically stirring the obtained mixture for 30 minutes, it was dried in a vacuum dryer and sealed.
실온 및 질소 가스 환경에서, 상기에서 얻어진 구리 파우더를 함유하는 결과물에 O-디메틸 에스터 에폭시 수지 90 중량부, 로우 메틸 에테르화 멜라민 포름알데하이드 수지 90 중량부, 폴리에테르 3.5 중량부, 메틸헥사하이드로프탈릭 무수물(methylhexahydrophthalic anhydride) 70 중량부, MY-24 4 중량부 및 나노 실리카 2 중량부를 연속으로 더하여 혼합물을 얻었다. 상기 혼합물을 균일하게 혼합하고, 진공 건조 오븐에 두어 기포를 제거함으로써, O-디메틸 에스터 에폭시 수지 도전성 접착제 D를 얻었다.In a room temperature and nitrogen gas environment, 90 parts by weight of O-dimethyl ester epoxy resin, 90 parts by weight of low methyl etherified melamine formaldehyde resin, 3.5 parts by weight of polyether, methylhexahydrophthalic in the resultant containing the copper powder obtained above. 70 parts by weight of methylhexahydrophthalic anhydride, 4 parts by weight of MY-24, and 2 parts by weight of nano silica were successively added to obtain a mixture. The mixture was uniformly mixed and placed in a vacuum drying oven to remove air bubbles, thereby obtaining an O-dimethyl ester epoxy resin conductive adhesive D.
실시예 5Example 5
구리 파우더 1000 중량부를 무게를 달아, 무수 에탄올에 용해된 KH550 20 중량부를 추가하였다. 얻어진 혼합물을 30분간 초음파 교반한 후, 진공 건조기에서 건조하고, 밀봉하였다.1000 parts by weight of copper powder was weighed, and 20 parts by weight of KH550 dissolved in absolute ethanol was added. After ultrasonically stirring the obtained mixture for 30 minutes, it was dried in a vacuum dryer and sealed.
실온 및 질소 가스 환경에서, 상기에서 얻어진 구리 파우더를 함유하는 결과물에 O-디메틸 에스터 에폭시 수지 100 중량부, 로우 메틸 에테르화 멜라민 포름알데하이드 수지 140 중량부, 폴리에테르 9 중량부, 메틸헥사하이드로프탈릭 무수물(methylhexahydrophthalic anhydride) 90 중량부, MY-24 6 중량부 및 나노 실리카 3 중량부를 연속으로 더하여 혼합물을 얻었다. 상기 혼합물을 균일하게 혼합하고, 진공 건조 오븐에 두어 기포를 제거함으로써, O-디메틸 에스터 에폭시 수지 도전성 접착제 E를 얻었다.In a room temperature and nitrogen gas environment, in the resultant product containing the copper powder obtained above, 100 parts by weight of O-dimethyl ester epoxy resin, 140 parts by weight of low methyl etherified melamine formaldehyde resin, 9 parts by weight of polyether, methylhexahydrophthalic 90 parts by weight of methylhexahydrophthalic anhydride, 6 parts by weight of MY-24, and 3 parts by weight of nano silica were successively added to obtain a mixture. The mixture was uniformly mixed and placed in a vacuum drying oven to remove air bubbles, thereby obtaining an O-dimethyl ester epoxy resin conductive adhesive E.
비교예 1Comparative Example 1
메틸헥사하이드로프탈릭 무수물과 경화 촉진제 MY-24 대신에 저분자 폴리아미드(low molecular polyamide)를 사용하고, 로우 메틸 에테르화 멜라민 포름알데하이드 수지와 폴리에테르 사용하지 않은 것을 제외하고, 실시예 1과 동일한 방법으로, O-디메틸 에스터 에폭시 수지 도전성 접착제 X를 준비하였다.The same method as in Example 1, except that low molecular polyamide was used instead of methylhexahydrophthalic anhydride and the curing accelerator MY-24, and low methyl etherified melamine formaldehyde resin and polyether were not used. As a result, an O-dimethyl ester epoxy resin conductive adhesive X was prepared.
비교예 2Comparative Example 2
나노 실리카를 사용하지 않은 것을 제외하고, 실시예 1과 동일한 방법으로, O-디메틸 에스터 에폭시 수지 도전성 접착제 Y를 준비하였다.In the same manner as in Example 1, except that nano silica was not used, an O-dimethyl ester epoxy resin conductive adhesive Y was prepared.
비교예 3Comparative Example 3
나노 실리카 5 중량부를 사용한 것을 제외하고, 실시예 1과 동일한 방법으로, O-디메틸 에스터 에폭시 수지 도전성 접착제 Z를 준비하였다.In the same manner as in Example 1, except that 5 parts by weight of nano silica was used, an O-dimethyl ester epoxy resin conductive adhesive Z was prepared.
평가 방법:Assessment Methods:
(1) 체적 저항률: GB/T1410-2006에 따라 평가하였다.(1) Volume resistivity: evaluated according to GB/T1410-2006.
(2) 전단 강도: GB/T 7124-2008에 따라, 평가를 위하여 본딩된 철 시트를 대기 중에 방치하여 20분간 실온에서 경화하였다.(2) Shear strength: According to GB/T 7124-2008, the bonded iron sheet for evaluation was allowed to stand in the air and cured at room temperature for 20 minutes.
(3) 보관 안정성: 얻어진 도전성 접착제를 5mL 투명 주사기에 넣고, 2달동안 실온에서 보관한 후, 겔화, 박리(delamination) 또는 침전(precipitation)을 시각적으로 검사하였다.(3) Storage stability: The obtained conductive adhesive was put into a 5 mL transparent syringe and stored at room temperature for 2 months, and then gelation, delamination or precipitation were visually inspected.
(4) 경화 시간: 상기 O-디메틸 에스터 에폭시 수지 도전성 접착제가 안정적인 체적 저항률과 안정적인 접착 강도를 갖는데 걸리는 시간을 측정하였다.(4) Curing time: The time taken for the O-dimethyl ester epoxy resin conductive adhesive to have a stable volume resistivity and stable adhesive strength was measured.
얻어진 결과들은 아래의 표 1에 나타내었다.The obtained results are shown in Table 1 below.
도전성 접착제
Conductive adhesive
경화시간(분)
Curing time (minutes)
체적 저항률
(Ω·m)
Volume resistivity
(Ω·m)
전단 강도(MPa)
Shear strength (MPa)
보관 안정성
(25℃，2개월)
Storage stability
(25℃, 2 months)
A
A
13
13
1.5×10- 6Ω·m
1.5 × 10 - 6 Ω · m
15.3
15.3
겔화/박리/침전 없음
No gelation/peel/precipitation
B
B
11
11
1.0×10- 6Ω·m
1.0 × 10 - 6 Ω · m
14.9
14.9
겔화/박리/침전 없음
No gelation/peel/precipitation
C
C
8
8
1.2×10- 6Ω·m
1.2 × 10 - 6 Ω · m
14.7
14.7
겔화/박리/침전 없음
No gelation/peel/precipitation
D
D
14
14
1.4×10- 6Ω·m
1.4 × 10 - 6 Ω · m
14.1
14.1
겔화/박리/침전 없음
No gelation/peel/precipitation
E
E
4
4
1.2×10- 6Ω·m
1.2 × 10 - 6 Ω · m
15.6
15.6
겔화/박리/침전 없음
No gelation/peel/precipitation
X
X
700
700
2.3×10- 6Ω·m
2.3 × 10 - 6 Ω · m
13.6
13.6
겔화 및 석출 발생
Gelation and precipitation occur
Y
Y
16
16
1.4×10- 6Ω·m
1.4 × 10 - 6 Ω · m
10
10
겔화/박리/침전 없음
No gelation/peel/precipitation
Z
Z
15
15
1.7×10- 6Ω·m
1.7 × 10 - 6 Ω · m
11.4
11.4
겔화/박리/침전 없음
No gelation/peel/precipitation
표 1을 참조하면, 본 발명의 경화 시스템을 채용한 도전성 접착제들은 실온에서 15분 이내에 빠르게 경화될 수 있으며, 본 발명의 경화 시스템을 채용하지 않은 도전성 접착제들에 비하여 개선된 전단 강도 및 보관 안정성을 가질 수 있음을 알 수 있다. 또한, 도전성 접착제 X-Z에 비하여, 본 발명에 따른 모든 도전성 접착제들은, 저하 없이 실질적으로 동일한 레벨로 체적 저항률이 유지됨을 알 수 있다.Referring to Table 1, the conductive adhesives employing the curing system of the present invention can be rapidly cured within 15 minutes at room temperature, and have improved shear strength and storage stability compared to the conductive adhesives not employing the curing system of the present invention. You can see that you can have it. In addition, compared to the conductive adhesive X-Z, it can be seen that the volume resistivity of all the conductive adhesives according to the present invention is maintained at substantially the same level without deterioration.
상술된 것들은 오직 본 발명의 실시예들이며, 이미 알려진 특정한 구조 및 성질들은 여기에 기술되지 않는다. 본 발명이 속하는 기술 분야의 통상의 지식을 가진 자라면 하기의 특허청구범위에 기재된 본 발명의 사상 및 영역으로부터 벗어나지 않는 범위 내에서 본 발명을 다양하게 수정 및 변경시킬 수 있으며, 이러한 모든 변형예들은 본 발명의 보호 범위 내에 있는 것으로 간주되어야 하며, 이들은 본 발명의 구현 효과와 특허 활용을 제한해서는 안된다. 본 출원에 의해 청구된 보호 범위는 청구항의 기재에 근거하여야 하며, 상세한 설명에 인용된 특정의 실시예들은 청구항의 기재를 설명하기 위한 것이다. Those described above are only embodiments of the present invention, and specific structures and properties already known are not described herein. Those of ordinary skill in the technical field to which the present invention pertains can variously modify and change the present invention without departing from the spirit and scope of the present invention described in the following claims, and all these modifications are It should be considered to be within the protection scope of the present invention, and these should not limit the implementation effect and patent application of the present invention. The scope of protection claimed by this application should be based on the description of the claims, and specific embodiments cited in the detailed description are intended to explain the description of the claims.
Claims (5)
로우 메틸 에테르화 멜라민 포름알데하이드 수지 50-150 중량부;
폴리에테르 2-10 중량부;
O-디메틸 에스터 에폭시 수지 경화제 50-90 중량부;
경화 촉진제 3-6 중량부;
구리 파우더 200-1600 중량부; 및
나노 실리카 2-4 중량부를 포함하고,
상기 구리 파우더는 실란 커플링제로 표면 개질되고,
실온에서 20분 이내에 경화 가능한, 실온 속경화형 도전성 접착제.100 parts by weight of O-dimethyl ester epoxy resin;
50-150 parts by weight of low methyl etherified melamine formaldehyde resin;
2-10 parts by weight of polyether;
O-dimethyl ester epoxy resin curing agent 50-90 parts by weight;
3-6 parts by weight of a hardening accelerator;
200-1600 parts by weight of copper powder; And
Including 2-4 parts by weight of nano silica,
The copper powder is surface modified with a silane coupling agent,
Room temperature fast curing type conductive adhesive that can be cured at room temperature within 20 minutes
The method of claim 1, wherein the conductive adhesive is 2 × 10 - in curing conductive adhesive, characterized in that has a lower volume resistivity than 6 and Ω m.
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2019
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