KR20090046513A - Pre-flux performing selective coating for pwb - Google Patents
Pre-flux performing selective coating for pwb Download PDFInfo
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- KR20090046513A KR20090046513A KR1020070112722A KR20070112722A KR20090046513A KR 20090046513 A KR20090046513 A KR 20090046513A KR 1020070112722 A KR1020070112722 A KR 1020070112722A KR 20070112722 A KR20070112722 A KR 20070112722A KR 20090046513 A KR20090046513 A KR 20090046513A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D235/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, condensed with other rings
- C07D235/02—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, condensed with other rings condensed with carbocyclic rings or ring systems
- C07D235/04—Benzimidazoles; Hydrogenated benzimidazoles
- C07D235/06—Benzimidazoles; Hydrogenated benzimidazoles with only hydrogen atoms, hydrocarbon or substituted hydrocarbon radicals, directly attached in position 2
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
Abstract
본 발명은 구리 또는 구리합금의 표면에 피막을 형성하기 위한 프리플럭스 조성물에 관한 것으로서, 자세하게는 경질 인쇄 배선판(PWB) 또는 가요성(flexible) 인쇄 배선판 상의 구리 또는 구리합금의 표면을 유기층을 형성시켜 보호하며 내열성이 뛰어나며, 구리표면에만 선택적으로 코팅되는 프리플럭스 조성물에 관한 것이다. 본 발명의 조성물의 구성은 벤즈이미다졸 유도체 0.5 ~ 3 g/L, 습윤제(wetting agent) 0.1 ~ 5 g/L, 유기산 또는 무기산 0.1 ~ 50 g/L, 킬레이트제 0.01 ~ 2 g/L, 구리 화합물 또는 철화합물 0.01 ~ 2 g/L, 나머지는 물로 이루어지고, pH가 2.7 ~ 3.3 인 것을 특징으로 한다. 본 발명에 의한 프리플럭스 조성물은 기존의 프리플럭스 조성물에 비하여 내열성이 높으며, 금 단자에는 코팅되지 않는 선택적 코팅성을 가지며, 향상된 납땜 습윤성을 가지는 프리플럭스 조성물을 제공한다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a preflux composition for forming a film on a surface of copper or a copper alloy, and in detail, an organic layer is formed on a surface of a copper or copper alloy on a rigid printed wiring board (PWB) or a flexible printed wiring board. It relates to a preflux composition which is protective and excellent in heat resistance and which is selectively coated only on the copper surface. The composition of the present invention is a benzimidazole derivative 0.5 ~ 3 g / L, wetting agent 0.1 ~ 5 g / L, organic acid or inorganic acid 0.1 ~ 50 g / L, chelating agent 0.01 ~ 2 g / L, copper Compound or iron compound 0.01 ~ 2 g / L, the rest is made of water, characterized in that the pH is 2.7 ~ 3.3. The preflux composition according to the present invention has a high heat resistance compared to the conventional preflux composition, has a selective coating property not coated on the gold terminal, and provides a preflux composition having improved solder wettability.
프리플럭스, 인쇄회로 배선판(PWB), 벤즈이미다졸계, 내열성, 납땜성, 금단자 Preflux, Printed Circuit Board (PWB), Benzimidazole Type, Heat Resistance, Solderability, Gold Terminal
Description
본 발명은 구리 또는 구리합금의 표면에 피막을 형성하기 위한 프리플럭스 조성물에 관한 것으로서, 자세하게는 경질 인쇄 배선판(PWB) 또는 가요성(flexible) 인쇄 배선판 상의 구리 또는 구리합금의 표면을 유기층을 형성시켜 보호하며 내열성이 뛰어나며, 구리표면에만 선택적으로 코팅되는 프리플럭스 조성물에 관한 것이다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a preflux composition for forming a film on a surface of copper or a copper alloy, and in detail, an organic layer is formed on a surface of a copper or copper alloy on a rigid printed wiring board (PWB) or a flexible printed wiring board. It relates to a preflux composition which is protective and excellent in heat resistance and which is selectively coated only on the copper surface.
인쇄 배선판의 구리 또는 구리합금으로 된 회로를 방청하고 납땜성을 유지하기 위한 방법으로는 회로를 납땜, 금, 팔라듐 등 다른 금속으로 피복하는 방법과 납땜코팅에 의한 방법, 유기피막을 피복하는 방법이 있다.Methods for rusting circuits made of copper or copper alloy on printed wiring boards and maintaining solderability include coating the circuits with other metals such as soldering, gold, and palladium, soldering coatings, and coating organic films. have.
프리플럭스는 인쇄 배선판(PWB)에 납땜이 이루어지는 회로배선의 산화를 방지하고 납땝성(solderability)을 유지시키기 위해 사용되는 표면처리제이다. 최근 인쇄배선판에 대한 전자부품의 접합방법으로서, 표면실장법(SMT)이 많이 이용되고, 부품장치의 앙면장착 또는 침부부품과 디스크리트 부품의 혼재 등에 의하여 인쇄배선판이 고온에 노출되기 때문에 인쇄배선판 상의 구리 회로를 보호하기 위해 프리 플럭스는 고내열성과 금단자에 코팅되지 않는 선택적 코팅성을 갖추어야 한다.Preflux is a surface treatment agent used to prevent oxidation of circuit wiring where solder is applied to a printed wiring board (PWB) and to maintain solderability. In recent years, as a method of bonding electronic components to printed wiring boards, surface mount method (SMT) is widely used, and since printed wiring boards are exposed to high temperatures due to face mounting of component devices or mixing of needle parts and discrete parts, copper on printed wiring boards is exposed. To protect the circuit, the preflux must have high heat resistance and an optional coating that is not coated on the metal terminals.
유기피막을 형성하는 재료에는 인쇄배선판 전체를 코팅하는 로진계 프리플럭스와 선택적으로 구리회로부에 화학반응으로 알킬이마다졸계 프리플러스가 있다.The materials for forming the organic coating include rosin-based preflux coating the entire printed wiring board and alkyl imidazole-based preplus by chemical reaction in the copper circuit part.
알킬이미다졸계 프리플럭스는 수용성이며, 작업환경이나 안전성의 면에서 우수하고, 실온에 가까운 온도에서 안정하지만, 고온에서는 비교적 단시간 내에 탈색이 일어나며 형성된 피막의 표면에서의 납땜이 편리하게 수행되지 않는 문제점이 있다.Alkylimidazole-based preflux is water-soluble, excellent in terms of working environment and safety, stable at temperatures close to room temperature, but at high temperatures, decolorization occurs within a short time, and soldering on the surface of the formed film is not easily performed. There is this.
따라서, 내열성이 불량한 알킬이미다졸계 프리플럭스를 대신하여, 벤즈이미다졸계 화합물을 유효 성분으로 하는 표면 처리제가 다수 개발되고 있는 실정이다. 대한민국 특허공개 제10-2004-0040857호의 인쇄배선판용 프리플럭스는 프리플럭스 용액의 침전화 방지와 내열성을 향상 시키는 프리플럭스 조성물이 개시되어 있고, 대한민국 특허공개 제10-1994-0026235호의 구리 및 구리합금의 표면처리제는 프리플럭스의 용액의 침전화를 방지하고, 침전되더라도 다시 쉽게 용해시킬수 있는 프리플럭스 조성물이 개시되어 있다. 또한, 대한민국 특허공개번호 제10-2002-7002389호의 구리기판의 선택적 침착방법에는 금의 전도성에 악영향이 미치지 않도록 인쇄기판용 회로에서 구리 표면상에 선택적으로 침착시키는 방법이 개시되어 있고, 대한민국 특허등록공고번호 제10-2005-0061166호의 프리플럭스 조성물에는 내열성이 향상되고 구리도금 회로에만 선택적으로 코팅될 수 있는 프리플럭스 조성물이 개시되어 있다. Therefore, many surface treatment agents which have a benzimidazole type compound as an active ingredient have been developed in place of the alkylimidazole type preflux having poor heat resistance. The preflux for printed wiring board of the Republic of Korea Patent Publication No. 10-2004-0040857 discloses a preflux composition for preventing precipitation of the preflux solution and improving heat resistance, and the copper and copper alloy of the Republic of Korea Patent Publication No. 10-1994-0026235 Surface treatment agents of the preflux to prevent the precipitation of the solution of the preflux, even if precipitated is disclosed a preflux composition that can be easily dissolved again. In addition, the method of selectively depositing a copper substrate of Korean Patent Publication No. 10-2002-7002389 discloses a method of selectively depositing on a copper surface in a printed circuit circuit so as not to adversely affect the conductivity of gold, and registered a Korean patent The preflux composition of Publication No. 10-2005-0061166 discloses a preflux composition which is improved in heat resistance and can be selectively coated only in a copper plating circuit.
상기 벤즈이미다졸계 화합물을 유효 성분으로 하는 표면처리제는 내열성이 다소 향상되었지만, 효과적인 표면실장(SMT)을 위해서는 255℃ 이상의 온도에서도 견딜수 있는 내열성을 가지는 것과 동시에 납땜습윤성의 향상이 필요로 하고, 구리표면의 산화방지를 위해 내습성 향상이 요구되어 지고 있다.The surface treatment agent containing the benzimidazole-based compound as an active ingredient is somewhat improved in heat resistance, but for effective surface mounting (SMT), it has heat resistance that can withstand temperatures of 255 ° C or higher, and at the same time, improves solder wettability, and copper In order to prevent oxidation of the surface, improvement of moisture resistance is required.
본 발명은 상기한 문제점을 해결하고자 안출된 것으로서, 기존의 프리플럭스 조성물에 비하여 내열성이 높으며, 금 단자에는 고팅되지 않는 선택적 코팅성을 가지며, 향상된 납땜 습윤성을 가지는 프리플럭스 조성물을 제공하는 데 있다. The present invention has been made to solve the above problems, and has a high heat resistance compared to the existing preflux composition, has a selective coating property that is not fixed to the gold terminal, to provide a preflux composition having improved solder wettability.
본 발명의 프리플럭스 조성물은 하기 화학식 1의 벤즈이미다졸 유도체 0.5 ~ 3 g/L, 습윤제(wetting agent) 0.1 ~ 5 g/L, 유기산 또는 무기산 0.1 ~ 50 g/L, 킬레이트제 0.01 ~ 2 g/L, 구리 화합물 또는 철화합물 0.01 ~ 2 g/L, 나머지는 물로이루어지고, pH가 2.7 ~ 3.3 이고, 구리 또는 구리합금에만 선택적으로 코팅되며, 납땜 습윤성이 우수하고 고내열성 특성을 가진다. Preflux composition of the present invention is a benzimidazole derivative of formula 1 0.5-3 g / L, wetting agent 0.1 ~ 5 g / L, organic or inorganic acid 0.1 ~ 50 g / L, chelating agent 0.01 ~ 2 g / L, copper compound or iron compound 0.01 ~ 2 g / L, the rest is made of water, the pH is 2.7 ~ 3.3, selectively coated only on copper or copper alloy, it has excellent soldering wettability and high heat resistance.
(상기 식에서 R1은 탄소가 1~10의 알킬기, 할로겐, 아릴기에서 선택되는 어느 하나이며, R2, R3는 각각 독립적으로 1개 이상의 탄소 알킬기에서 선택되는 어느하나이다.)(In the formula, R1 is any one selected from the alkyl group of 1 to 10 carbon atoms, halogen, aryl group, R2, R3 are each independently selected from one or more carbon alkyl groups.)
상기 벤즈이미다졸 유도체는 2-메틸벤즈이미다졸, 2-프로필벤즈이미다졸, 2-부틸벤즈이미다졸, 2-펜틸벤즈이미다졸, 2-헥실벤즈이미다졸, 2-헵틸벤즈이미다졸, 2-옥틸벤즈이미다졸, 2-노닐벤즈이미다졸, 2-(4-벤질)벤즈이미다졸, 2-(3-페닐프로필)벤즈이미다졸, 2-(4-페닐부틸)벤즈이미다졸, 2-(5-페닐펜틸)벤즈이미다졸, 2-(6-페닐헥실)벤즈이미다졸, 2-(8-페닐헵틸)벤즈이미다졸, 2-(8-페닐옥틸)벤즈이미다졸, 2-(9-페닐노닐)벤즈이미다졸, 2-(10-페닐데실)벤즈이미다졸, 2-벤질-4-메틸벤즈이미다졸, 4-메틸-2-페닐에틸벤즈이미다졸, 4-메틸-2-(3-페닐프로필)벤즈이미다졸, 4-메틸-2-(5-페닐펜틸)벤즈이미다졸, 4-메틸-2-(6-페닐펜틸)벤즈이미다졸, 4-메틸-2-(8-페닐옥틸)벤즈이미다졸 및 그들의 염들 중에서 선택되는 어느 하나 이상으로 이루어진다. The benzimidazole derivatives are 2-methylbenzimidazole, 2-propylbenzimidazole, 2-butylbenzimidazole, 2-pentylbenzimidazole, 2-hexylbenzimidazole, 2-heptylbenzimidazole, 2- Octylbenzimidazole, 2-nonylbenzimidazole, 2- (4-benzyl) benzimidazole, 2- (3-phenylpropyl) benzimidazole, 2- (4-phenylbutyl) benzimidazole, 2- ( 5-phenylpentyl) benzimidazole, 2- (6-phenylhexyl) benzimidazole, 2- (8-phenylheptyl) benzimidazole, 2- (8-phenyloctyl) benzimidazole, 2- (9- Phenylnonyl) benzimidazole, 2- (10-phenyldecyl) benzimidazole, 2-benzyl-4-methylbenzimidazole, 4-methyl-2-phenylethylbenzimidazole, 4-methyl-2- (3 -Phenylpropyl) benzimidazole, 4-methyl-2- (5-phenylpentyl) benzimidazole, 4-methyl-2- (6-phenylpentyl) benzimidazole, 4-methyl-2- (8-phenyl Octyl) benzimidazole and their salts.
상기 습윤제(wetting agent)는 부톡시에탄올, 에틸렌 글리콜, 팬타노익, 헵타노익, 소듐 설포다이메틸 아이소프탈레이트, 모노글설페이드 중에 선택되는 어느 하나 이상으로 이루어진다.The wetting agent (wetting agent) is composed of any one or more selected from butoxyethanol, ethylene glycol, pananoic, heptanoic, sodium sulfodimethyl isophthalate, monosulfide.
상기 유기산 또는 무기산은 구연산, 주석산, 빙초산, 젖산, 벤조산, 개미산, 프로피온산, 아크릴산, 부틸릭산, 파미틱산, 스테아르산 중에서 선택되는 어느 하나 이상의 유기산, 또는 황산, 질산, 인산, 염산, 탄산 중에서 선택되는 어느 하나 이상의 무기산으로 이루어진다.The organic acid or inorganic acid is any one or more organic acids selected from citric acid, tartaric acid, glacial acetic acid, lactic acid, benzoic acid, formic acid, propionic acid, acrylic acid, butyric acid, paretic acid, stearic acid, or sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, and carbonic acid. It consists of any one or more inorganic acids.
상기 킬레이트제는 니트릴로트리아세틱에시드(NTA), 에틸렌디아민테트라아세틱에시드(EDTA). 시트르산, 굴루코산, 폴리인산 중에서 선택되는 하나 이상으로 이루어진다.The chelating agent is nitrilotriacetic acid (NTA), ethylenediaminetetraacetic acid (EDTA). It consists of one or more selected from citric acid, gurucoic acid, polyphosphoric acid.
상기 구리화합물 또는 철화합물은 염화제1구리, 염화제2구리, 염화제3구리, 황산구리, 질신구리 중에서 선택되는 어느 하나 이상의 구리화합물 또는 염화제1철, 염화제2철, 염화제3철 중에서 선택되는 어느 하나 이상의 철화합물로 이루어진다 The copper compound or iron compound is any one or more of the copper compound selected from cuprous chloride, cupric chloride, cupric chloride, cupric sulfate, cuprous nitrate or ferric chloride, ferric chloride, ferric chloride Consists of any one or more iron compounds selected
본 발명에 따른 프리플럭스 조성물을 사용하는 경우, 기존의 프리플럭스 보다 향상된 내열성을 가지게 되어 납땜 뿐만 아니라, 납땜 대체용 합금을 이용하는 경우에도 사용될 수 있으며, 구리도금회로에 선택적으로 코팅될 수 있기 때문에 금도금회로에 코팅 얼룩으로 인한 전도성 감소를 배제할 수 있고, 납땜 습윤성과 내습성으로 인해 인쇄배선판 회로에 안정적인 코팅막을 형성할 수 있다.In the case of using the preflux composition according to the present invention, it has improved heat resistance than the conventional preflux and can be used not only for soldering, but also for the use of an alloy for soldering replacement and gold plating because it can be selectively coated on a copper plating circuit. The reduction in conductivity due to coating stains in the circuit can be eliminated, and the solder wettability and moisture resistance can form a stable coating on the printed circuit board circuit.
이하 본 발명의 프리플럭스 조성물에 대하여 자세히 설명한다.Hereinafter, the preflux composition of the present invention will be described in detail.
본 발명의 프리플럭스 조성물은 벤즈이미다졸 유도체 0.5 ~ 3 g/L, 습윤제(wetting agent) 0.1 ~ 5 g/L, 유기산 또는 무기산 0.1 ~ 50 g/L, 킬레이트제 0.01 ~ 2 g/L, 구리 화합물 또는 철화합물 0.01 ~ 2 g/L, 나머지는 물로 이루어지고, pH가 2.7 ~ 3.3 인 것을 특징으로 하는 납땜 습윤성이 우수하고 구리 또는 구리도금 회로에 선택적 코팅이 가능한 고내열성 프리플럭스 조성물이다.Preflux composition of the present invention is a benzimidazole derivative 0.5 to 3 g / L, wetting agent 0.1 to 5 g / L, organic or inorganic acid 0.1 to 50 g / L, chelating agent 0.01 to 2 g / L, copper Compound or iron compound 0.01 ~ 2 g / L, the rest is made of water, the pH is 2.7 ~ 3.3 is a high heat resistance preflux composition capable of excellent solder wettability and selective coating on the copper or copper plating circuit.
상기 벤즈이마다졸 유도체는 예를 들어, 상기 벤즈이미다졸 유도체는 2-메틸벤즈이미다졸, 2-프로필벤즈이미다졸, 2-부틸벤즈이미다졸, 2-펜틸벤즈이미다졸, 2-헥실벤즈이미다졸, 2-헵틸벤즈이미다졸, 2-옥틸벤즈이미다졸, 2-노닐벤즈이미다 졸, 2-(4-벤질)벤즈이미다졸, 2-(3-페닐프로필)벤즈이미다졸, 2-(4-페닐부틸)벤즈이미다졸, 2-(5-페닐펜틸)벤즈이미다졸, 2-(6-페닐헥실)벤즈이미다졸, 2-(8-페닐헵틸)벤즈이미다졸, 2-(8-페닐옥틸)벤즈이미다졸, 2-(9-페닐노닐)벤즈이미다졸, 2-(10-페닐데실)벤즈이미다졸, 2-벤질-4-메틸벤즈이미다졸, 4-메틸-2-페닐에틸벤즈이미다졸, 4-메틸-2-(3-페닐프로필)벤즈이미다졸, 4-메틸-2-(5-페닐펜틸)벤즈이미다졸, 4-메틸-2-(6-페닐펜틸)벤즈이미다졸, 4-메틸-2-(8-페닐옥틸)벤즈이미다졸 및 그들의 염들 중에서 선택되는 어느 하나 이상을 선택하여 0.5~3 g/L를 사용하는 것이 바람직하며, 더욱 바람직하게는 1~2 g/L를 사용한다. 벤즈이미다졸 유도체의 함량이 0.5 g/L 미만인 경우 유효성분 함량이 낮아져서 인쇄회로 배선판의 구리 및 구리합금에 피막이 형성되지 않으며, 3 g/L 초과인 경우 유효성분의 함량이 너무 높아서 코팅 피막이 높게 형성되게 되고 납땜성 저해 요인으로 작용하게 된다.The benzimidazole derivatives are, for example, the benzimidazole derivatives are 2-methylbenzimidazole, 2-propylbenzimidazole, 2-butylbenzimidazole, 2-pentylbenzimidazole, 2-hexylbenzimidazole , 2-heptylbenzimidazole, 2-octylbenzimidazole, 2-nonylbenzimidazole, 2- (4-benzyl) benzimidazole, 2- (3-phenylpropyl) benzimidazole, 2- (4 -Phenylbutyl) benzimidazole, 2- (5-phenylpentyl) benzimidazole, 2- (6-phenylhexyl) benzimidazole, 2- (8-phenylheptyl) benzimidazole, 2- (8-phenyl Octyl) benzimidazole, 2- (9-phenylnonyl) benzimidazole, 2- (10-phenyldecyl) benzimidazole, 2-benzyl-4-methylbenzimidazole, 4-methyl-2-phenylethylbenz Imidazole, 4-methyl-2- (3-phenylpropyl) benzimidazole, 4-methyl-2- (5-phenylpentyl) benzimidazole, 4-methyl-2- (6-phenylpentyl) benzimidazole , At least one selected from 4-methyl-2- (8-phenyloctyl) benzimidazole and salts thereof To select it preferred to use 0.5 ~ 3 g / L, and use even more preferably 1 ~ 2 g / L. If the content of the benzimidazole derivative is less than 0.5 g / L, the active ingredient content is lowered, so that the coating is not formed on the copper and copper alloy of the printed circuit board. If the content of the benzimidazole derivative is higher than 3 g / L, the coating layer is formed because the active ingredient is too high. This will act as a deterrent to solderability.
상기 벤즈이미다졸 유도체는 물에 대하여 난용성이므로 이를 물에 용해시키기 위해 유기산 또는 무기산 사용하여 가용화하며, 산으로는 구연산, 주석산, 빙초산, 젖산, 벤조산, 개미산, 프로피온산, 아크릴산, 부틸릭산, 팔미틱산, 스테아르산 등이 이용되며, 무기산은 황산, 질산, 인산, 염산, 탄산 등에서 하나 또는 이들의 혼합물을 사용한다. 함량은 0.1~50 g/L를 사용하는 것이 바람직하다. 유기산 또는 무기산의 함량이 0.1 g/L 미만의 경우 프리플럭스 조성물의 유요성분인 벤즈이미다졸 유도체가 석출이 발생하여 유효성분이 현저히 줄어들고, 50 g/L 초과의 경우 인쇄회로 배선판의 구리 및 구리합금 코팅 피막이 얇게 형성되어 내열성을 갖추지 못하게 된다.Since the benzimidazole derivative is poorly soluble in water, it is solubilized using an organic acid or an inorganic acid to dissolve it in water. As the acid, citric acid, tartaric acid, glacial acetic acid, lactic acid, benzoic acid, formic acid, propionic acid, acrylic acid, butyric acid, and palmitic acid are used. , Stearic acid and the like are used, and the inorganic acid uses one or a mixture thereof in sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, carbonic acid and the like. It is preferable to use content 0.1-50 g / L. If the content of organic acid or inorganic acid is less than 0.1 g / L, the benzimidazole derivative, an active ingredient of the preflux composition, is precipitated and the active ingredient is significantly reduced, and if it is more than 50 g / L, the copper and copper alloy coating of the printed circuit board The film is formed thin so that it does not have heat resistance.
상기 습윤제(Wetting agent)는 친수성기와 소수성기를 가지고 있어 코팅 표면의 소수성기에 의해 방습효과를 나타내게 할 수 있으며, 코팅 피막의 납땜 습윤성을 향상시키게 된다. 습윤제로 는 부톡시에탄올, 에틸렌 글리콜, 펜타노익, 헵타노익, 소듐 설포다이메틱 아이소프탈레이트, 모노글리설페이드 중 선택되는 하나 이상이 사용된다. 습윤제의 함량은 0.1~5 g/L를 사용하는 것이 바람직하며, 더욱 바람직하게는 1~3 g/L를 사용한다. 습윤제의 함량이 0.1 g/L 이하의 경우, 인쇄회로 배선판의 구리 및 구리합금의 코팅피막 표면이 고르지 못하게 되며, 5 g/L 이상의 경우 코팅 피막 표면에 얼룩과 이물질이 뭍어 나오면서 프리플럭스의 안정성이 떨어진다.The wetting agent (wetting agent) has a hydrophilic group and a hydrophobic group can exhibit a moisture-proof effect by the hydrophobic group on the surface of the coating, and improve the solder wettability of the coating film. As the wetting agent, at least one selected from butoxyethanol, ethylene glycol, pentanoic, heptanoic, sodium sulfodimeric isophthalate, and monoglysulfide is used. The content of the humectant is preferably 0.1 to 5 g / L, more preferably 1 to 3 g / L. If the content of the wetting agent is 0.1 g / L or less, the surface of the coating film of copper and copper alloy of the printed circuit board becomes uneven. If the content of the wetting agent is more than 5 g / L, the surface of the coating film is smeared and foreign matters to prevent preflux stability. Falls.
킬레이트제는 구리 및 구리도금 회선의 선택적 코팅과 관련된 성분으로서, 에틸렌 디아민 테트라아세틱에시드(EDTA), 니트릴로트리아세틱에시드(NTA), 시트르산, 굴루코산, 폴리인산 들 중에 하나 이상이 사용된다. 상기 킬레이트제의 함량은 0.01~2 g/L를 사용하는 것이 바람직하며, 더욱 바람직하게는 0.5~1.5 g/L를 사용한다. 상기 킬레이트제의 함량이 0.01 g/L 미만의 경우 인쇄회로 배선판의 금 단자 부분에 얼룩이 발생하게 되며, 2 g/L 초과의 경우, 인쇄회로 배선판의 구리 및 구리합금에 피막이 얇게 되며, 얼룩이 발생한다.Chelating agents are components associated with the selective coating of copper and copper plated lines, and at least one of ethylene diamine tetraacetic acid (EDTA), nitrilotriacetic acid (NTA), citric acid, gulucoic acid, polyphosphoric acid is used. The content of the chelating agent is preferably used from 0.01 to 2 g / L, more preferably from 0.5 to 1.5 g / L. If the content of the chelating agent is less than 0.01 g / L, staining occurs on the gold terminal portion of the printed circuit board, and when it exceeds 2 g / L, the coating film becomes thin on the copper and copper alloy of the printed circuit board, and staining occurs. .
구리 화합물 또는 철화합물은 염화제1구리, 염화제2구리, 염화제3구리, 황산구리, 질산구리, 염화 제1철, 염화제2철, 염화제3철 중에서 하나 이상이 선택되어 사용되며, 함량은 0.01~2 g/L를 사용하는 것이 바람직하다. 구리 화합물 또는 철화합물의 함량이 0.01 g/L를 초과하는 경우 인쇄회로기판의 구리 및 구리합금에 코팅 피막의 내열성이 약해지며, 2 g/L 초과의 경우 인쇄회로기판의 금단자에 이물질이 발생하여 불량의 요인이 된다.The copper compound or iron compound is selected from at least one of cuprous chloride, cupric chloride, cupric chloride, copper sulfate, copper nitrate, ferrous chloride, ferric chloride, and ferric chloride. It is preferable to use 0.01-2 g / L of silver. When the content of copper compound or iron compound exceeds 0.01 g / L, the heat resistance of the coating film is weakened on the copper and copper alloy of the printed circuit board, and when it exceeds 2 g / L, foreign matter occurs on the gold terminal of the printed circuit board. This is a cause of failure.
본 발명의 프리플럭스 조성물의 pH는 2.3 ~ 4 로 유지하는 것이 바람직하다. pH가 2.3 미만의 경우 인쇄회로배선판의 구리 및 구리 합금에 피막이 형성되는 속도가 현저하게 감소하여 코팅이 잘 일어나지 않으며, pH가 4 초과의 경우 피막 두계가 높게 형성되어 납땜성에서 문제가 발생하며, 벤조이미다졸 유도체의 석출이 발생한다.It is preferable to maintain pH of the preflux composition of this invention at 2.3-4. If the pH is less than 2.3, the formation rate of the film on the copper and copper alloy of the printed circuit board is significantly reduced, so that the coating does not occur well. If the pH is higher than 4, the film thickness is formed high, which causes problems in solderability. Precipitation of benzoimidazole derivatives occurs.
본 발명의 프리플럭스 조성물은 구리와 금이 혼재된 쿠폰을 이용하여, 탈지, 소프트 에칭, 산세 등을 처리한 후에 25~50℃ 온도범위로 10~120초에 걸쳐 접촉시킬 수 있다.The preflux composition of the present invention may be contacted over a temperature range of 25 to 50 ° C. over 10 to 120 seconds after degreasing, soft etching, and pickling using a coupon in which copper and gold are mixed.
이하 본 발명의 구체적인 설명을 위하여 실시예를 들어 설명한다. 본 발명이 실시예에 의하여 한정되는 것은 아니다.Hereinafter will be described with reference to the embodiment for a specific description of the invention. The present invention is not limited by the examples.
하기 실험조건에 따라 측정한 코팅두께, 부식여부, 내열성상태, 납오름성, 금단자 반응여부에 대해서 표1에 나타내었다.Table 1 shows the coating thickness, corrosion status, heat resistance, lead resistance, and gold terminal reaction measured according to the following experimental conditions.
<발명예 1>Invention Example 1
2-벤질-4-메틸벤즈이미다졸 1.5g/L, 빙초산 30g/L, 염화철 1g/L, NTA 0.5 g/L, 에틸렌 글리콜 2g/L를 첨가하고 프리플럭스 조성물이 1L가 되도록 물을 첨가하여 교반한 후 pH를 2.7이 되도록 한다.1.5 g / L of 2-benzyl-4-methylbenzimidazole, 30 g / L of glacial acetic acid, 1 g / L of iron chloride, 0.5 g / L of NTA, 2 g / L of ethylene glycol were added and water was added so that the preflux composition was 1 L. After stirring, the pH is brought to 2.7.
이 후에 탈지, 소프트 액칭 처리한 구리와 금이 혼재된 쿠폰을 액 온도 35℃에서 침지한 후 꺼내여 열풍으로 건조하였다. 구리 쿠폰의 코팅 두께는 0.25㎛가 측정되었고 금 단자는 미코팅이 되었다.After this, the coupon mixed with degreasing and soft quenching copper and gold was immersed at a liquid temperature of 35 ° C., and then taken out and dried by hot air. The coating thickness of the copper coupon was measured 0.25 탆 and the gold terminals were uncoated.
납땜 습윤성을 측정하기 위해서 상기 구리와 금이 혼재된 쿠폰을 온도 85℃, 습도 85%에서 유지 되는 열경화조 내에서 360시간 동안 방치 시켰을 때, 코팅된 구리표면의 상태를 보았다. 코팅된 곳은 전혀 부식의 흔적이 없었다.In order to measure the solder wettability, when the coupon containing the mixed copper and gold was left in a thermosetting tank maintained at a temperature of 85 ° C. and a humidity of 85% for 360 hours, the state of the coated copper surface was observed. The coated area had no signs of corrosion at all.
또한 상기 코팅된 구리 쿠폰의 내열성 상태 Test을 위해서 Reflow Test를 실시 하였다. Reflow 온도는 265℃에서 3번 처리 했을 때, 상기 코팅된 구리 쿠폰의 상태는 양호 하였고, 이 구리 쿠폰에 포스트 플럭스를 바른 후에 온도 270℃ 납땜조에 침지 하였다. 수초 후에 꺼내어 관찰한 결과 납오름성은 우수 하였다.In addition, a reflow test was performed to test the heat resistance of the coated copper coupon. When the reflow temperature was treated three times at 265 ° C., the coated copper coupon was in good condition, and after the post flux was applied to the copper coupon, it was immersed in a soldering bath at a temperature of 270 ° C. After a few seconds, the lead rise was excellent.
<발명예 2>Invention Example 2
상기 발명예 1에서 에틸렌 글리콜 대신에 모노글리설페이드 3g/L을 사용한 것을 제외하고는 동일한 조건으로 조성물을 만들어 발명예 1과 동일한 방법으로 처리하여 실시하였다. 이와 같이 얻은 구리와 금이 혼재된 쿠폰에서 코팅된 구리의 두께는 0.3㎛가 측정 되었고 금 단자는 미코팅이 되었다. Except for using ethylene glycol monoglycol sulfate instead of 3g / L in Inventive Example 1, the composition was prepared under the same conditions and treated in the same manner as Inventive Example 1. In the coupon obtained by mixing the copper and gold thus obtained, the thickness of the coated copper was measured to 0.3㎛ and the gold terminal was uncoated.
또한 상기 코팅된 구리 쿠폰의 내열성 상태 Test을 위해서 Reflow Test를 실시 하였다. Reflow 온도는 265℃에서 3번 처리 했을 때, 상기 코팅된 구리 쿠폰의 상태는 양호 하였고, 이 구리 쿠폰에 포스트 플럭스를 바른 후에 온도 270℃ 납땜조에 침지 하였다. 수초 후에 꺼내어 관찰한 결과 납오름성은 우수 하였다.In addition, a reflow test was performed to test the heat resistance of the coated copper coupon. When the reflow temperature was treated three times at 265 ° C., the coated copper coupon was in good condition, and after the post flux was applied to the copper coupon, it was immersed in a soldering bath at a temperature of 270 ° C. After a few seconds, the lead rise was excellent.
<발명예 3>Invention Example 3
상기 발명예 1에서 에틸렌 글리콜 대신에 팬타노익 2.5g/L을 사용한 것을 제외하고는 동일한 조건으로 조성물을 만들어 발명예 1과 동일한 방법으로 처리하 여 실시하였다. 이와 같이 얻은 구리와 금이 혼재된 쿠폰에서 코팅된 구리의 두께는 0.33㎛가 측정 되었고 금 단자는 미코팅이 되었다. Except for using ethylene glycol Pantanic 2.5g / L instead of ethylene glycol in the Inventive Example 1, the composition was prepared under the same conditions and treated in the same manner as Inventive Example 1. The thickness of the copper coated in the copper and gold coupons thus obtained was measured 0.33㎛ and the gold terminal was uncoated.
또한 상기 코팅된 구리 쿠폰의 내열성 상태 Test을 위해서 Reflow Test를 실시 하였다. Reflow 온도는 265℃에서 3번 처리 했을 때, 상기 코팅된 구리 쿠폰의 상태는 양호 하였고, 이 구리 쿠폰에 포스트 플럭스를 바른 후에 온도 270℃ 납땜조에 침지 하였다. 수초 후에 꺼내어 관찰한 결과 납오름성은 우수하였다.In addition, a reflow test was performed to test the heat resistance of the coated copper coupon. When the reflow temperature was treated three times at 265 ° C., the coated copper coupon was in good condition, and after the post flux was applied to the copper coupon, it was immersed in a soldering bath at a temperature of 270 ° C. After a few seconds, the lead rise was excellent.
<비교예 1>Comparative Example 1
물 1ℓ에 2-(5-페닐펜틸)벤즈이미다졸 5g/L, 구연산 40g/L, 염화철 3g/L, 시트르산 3g/L, 에틸렌 글리콜 0.05g/L 교반한 후 pH를 2.7이 되도록 한다. 이 후에 탈지, 소프트 액칭 처리한 구리와 금이 혼재된 쿠폰을 액 온도 35℃에서 침지한 후 꺼내여 열풍으로 건조하였다. 구리 쿠폰의 코팅 두께는 0.23㎛가 측정되었고 금 단자에 코팅이 되었다.5 g / L of 2- (5-phenylpentyl) benzimidazole, 40 g / L of citric acid, 3 g / L of iron chloride, 3 g / L of citric acid, and 0.05 g / L of ethylene glycol were stirred in 1 L of water, and the pH was adjusted to 2.7. After this, the coupon mixed with degreasing and soft quenching copper and gold was immersed at a liquid temperature of 35 ° C., and then taken out and dried by hot air. The coating thickness of the copper coupon was measured 0.23 μm and coated on the gold terminals.
납땜 습윤성을 측정하기 위해서 상기 구리와 금이 혼재된 쿠폰을 온도 85℃, 습도 85%에서 유지 시켜 코팅된 구리표면의 상태를 보았다. 코팅된 곳은 부식되었다.In order to measure the solder wettability, the copper and gold mixed coupons were maintained at a temperature of 85 ° C. and a humidity of 85% to observe the state of the coated copper surface. The coated area was corroded.
상기 코팅된 구리 쿠폰의 내열성 상태 Test을 위해서 Reflow Test를 실시 하였다. Reflow 온도는 265℃에서 3번 처리 했을 때, 상기 코팅된 구리 쿠폰의 상태는 열산화가 되었으며, 이 구리 쿠폰에 포스트 플럭스를 바른 후에 온도 270℃ 납땜조에 침지 하였다. 수초 후에 꺼내어 관찰한 결과 납오름성은 매우 나빴다.Reflow test was performed to test the heat resistance of the coated copper coupon. When the reflow temperature was treated three times at 265 ° C., the coated copper coupon was thermally oxidized. After applying the post flux to the copper coupon, it was immersed in a soldering bath at a temperature of 270 ° C. After a few seconds, the lead rise was very bad.
<비교예 2>Comparative Example 2
2-(3-페닐프로필)벤즈이미다졸 5g/L, 빙초산 40g/L, 염화철 0.005g/L, 부톡시에탄올 5g/L를 첨가하고 프리플럭스 조성물이 1L가 되도록 물을 첨가하여 pH를 3.5이 되도록 한다. 이 후에 탈지, 소프트 액칭 처리한 구리와 금이 혼재된 쿠폰을 액 온도 35℃에서 침지한 후 꺼내여 열풍으로 건조하였다. 구리 쿠폰의 코팅 두께는 0.5㎛가 측정되었고 금 단자에 코팅이 되었다.5 g / L of 2- (3-phenylpropyl) benzimidazole, 40 g / L of glacial acetic acid, 0.005 g / L of iron chloride, and 5 g / L of butoxyethanol were added and water was added so that the preflux composition was 1 L. Be sure to After this, the coupon mixed with degreasing and soft quenching copper and gold was immersed at a liquid temperature of 35 ° C., and then taken out and dried by hot air. The coating thickness of the copper coupon was measured 0.5 mu m and coated on the gold terminal.
납땜 습윤성을 측정하기 위해서 상기 구리와 금이 혼재된 쿠폰을 온도 85℃, 습도 85%에서 유지 시켜 코팅된 구리표면의 상태를 보았다. 코팅된 곳은 양호하였다.In order to measure the solder wettability, the copper and gold mixed coupons were maintained at a temperature of 85 ° C. and a humidity of 85% to observe the state of the coated copper surface. The coated place was good.
상기 코팅된 구리 쿠폰의 내열성 상태 Test을 위해서 Reflow Test를 실시 하였다. Reflow 온도는 265℃에서 3번 처리 했을 때, 상기 코팅된 구리 쿠폰의 상태는 양호 하였고, 이 구리 쿠폰에 포스트 플럭스를 바른 후에 온도 270℃ 납땜조에 침지 하였다. 수초 후에 꺼내어 관찰한 결과 납오름성은 매우 나빴다.Reflow test was performed to test the heat resistance of the coated copper coupon. When the reflow temperature was treated three times at 265 ° C., the coated copper coupon was in good condition, and after the post flux was applied to the copper coupon, it was immersed in a soldering bath at a temperature of 270 ° C. After a few seconds, the lead rise was very bad.
<비교예 3>Comparative Example 3
물 1ℓ에 2-(3-페닐프로필)벤즈이미다졸 0.2g/L, 빙초산 40g/L, 염화철 4g/L 부톡시에탄올 5g/L를 교반한 후 pH를 3.0이 되도록 한다. 이 후에 탈지, 소프트 액칭 처리한 구리와 금이 혼재된 쿠폰을 액 온도 35℃에서 침지한 후 꺼내여 열풍으로 건조하였다. 구리 쿠폰의 코팅 두께는 0.15㎛가 측정되었고 금 단자에 코팅이 되었다.To 1 liter of water, 0.2 g / L of 2- (3-phenylpropyl) benzimidazole, 40 g / L of glacial acetic acid, 4 g / L of iron chloride, and 5 g / L of butoxyethanol were stirred, and the pH was adjusted to 3.0. After this, the coupon mixed with degreasing and soft quenching copper and gold was immersed at a liquid temperature of 35 ° C., and then taken out and dried by hot air. The coating thickness of the copper coupon was measured 0.15 μm and coated on the gold terminals.
납땜 습윤성을 측정하기 위해서 상기 구리와 금이 혼재된 쿠폰을 온도 85℃, 습도 85%에서 유지 시켜 코팅된 구리표면의 상태를 보았다. 코팅된 곳은 부식되었 다.In order to measure the solder wettability, the coupon containing the copper and gold was kept at a temperature of 85 ° C. and a humidity of 85% to observe the state of the coated copper surface. The coated area was corroded.
상기 코팅된 구리 쿠폰의 내열성 상태 Test을 위해서 Reflow Test를 실시 하였다. Reflow 온도는 265℃에서 3번 처리 했을 때, 상기 코팅된 구리 쿠폰의 상태는 열산화 되었고, 이 구리 쿠폰에 포스트 플럭스를 바른 후에 온도 270℃ 납땜조에 침지 하였다. 수초 후에 꺼내어 관찰한 결과 납오름성은 매우 나빴다.Reflow test was performed to test the heat resistance of the coated copper coupon. When the reflow temperature was treated three times at 265 ° C., the state of the coated copper coupon was thermally oxidized. After applying the post flux to the copper coupon, the reflow temperature was immersed in a soldering bath at a temperature of 270 ° C. After a few seconds, the lead rise was very bad.
<종례예 1><Example 1>
2-헵틸벤즈이미다졸 5g, 개미산 20g, 염화철 0.2g, 에틸렌디아민 3초산 0.3g, 질산니켈 1g, 요오드화칼륨 5g을 첨가하고 프리플럭스 조성물이 1L가 되도록 물을 첨가하여 충분히 교반한 후, pH 2.9가 되도록 한다. 이 후에 탈지, 소프트 에칭 처리한 구리와 금이 혼재된 쿠폰을 액 온도 40℃에서 침지한 후 꺼내어 열풍으로 건조하였다. 이와 같이 하여 얻은 시험편 표면의 코팅 두께는 0.3㎛이었으나, 금 단자에 코팅이 되는 문제가 발견되었다.5 g of 2-heptylbenzimidazole, 20 g of formic acid, 0.2 g of iron chloride, 0.3 g of ethylenediamine triacetic acid, 1 g of nickel nitrate, and 5 g of potassium iodide are added, and water is sufficiently stirred until the preflux composition is 1 L, followed by pH 2.9 To be After this, the coupon mixed with copper and gold degreased and soft-etched was immersed at a liquid temperature of 40 ° C., and then taken out and dried by hot air. Although the coating thickness of the test piece surface obtained in this way was 0.3 micrometer, the problem which coated on a gold terminal was discovered.
<종례예 2><Example 2>
종례예 1 에서 염화철 대신 염화구리 0.2g을 사용한 것을 제외하고는 동일한 조건으로 수용액을 제조하여 종례예 1과 동일한 방법으로 처리를 수행하였다. An aqueous solution was prepared under the same conditions as in Example 1 except that 0.2 g of copper chloride was used instead of iron chloride, and the same treatment as in Example 1 was performed.
이와 같이 하여 얻은 시험편 표면의 코팅 두께는 0.3㎛이었으나, 금 단자에 코팅이 되는 문제가 발생하였다.Although the coating thickness of the test piece surface obtained in this way was 0.3 micrometer, the problem which coated on a gold terminal generate | occur | produced.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR102298998B1 (en) * | 2021-01-19 | 2021-09-07 | 백승룡 | Organic coating agent for surface treatment of plating layer containing copper and surface treatment of plating layer using the same |
| CN114833491A (en) * | 2022-06-21 | 2022-08-02 | 广东哈福科技有限公司 | Copper surface selective organic solderability preservative and use method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR102298998B1 (en) * | 2021-01-19 | 2021-09-07 | 백승룡 | Organic coating agent for surface treatment of plating layer containing copper and surface treatment of plating layer using the same |
| CN114833491A (en) * | 2022-06-21 | 2022-08-02 | 广东哈福科技有限公司 | Copper surface selective organic solderability preservative and use method thereof |
| CN114833491B (en) * | 2022-06-21 | 2024-04-30 | 广东哈福技术股份有限公司 | Copper surface selective organic soldering flux and use method thereof |
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