KR100765192B1 - Synthesis of organic silver solution - Google Patents

Synthesis of organic silver solution Download PDF

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KR100765192B1
KR100765192B1 KR1020060040833A KR20060040833A KR100765192B1 KR 100765192 B1 KR100765192 B1 KR 100765192B1 KR 1020060040833 A KR1020060040833 A KR 1020060040833A KR 20060040833 A KR20060040833 A KR 20060040833A KR 100765192 B1 KR100765192 B1 KR 100765192B1
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solution
acid
organic silver
dissolved
silver
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김동표
최윤혁
김현정
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주식회사 엔피케이
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • 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
    • C09D11/00—Inks
    • C09D11/30—Inkjet printing inks
    • 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
    • C09D11/00—Inks
    • C09D11/52—Electrically conductive inks
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K1/00—Printed circuits
    • H05K1/02—Details
    • H05K1/09—Use of materials for the conductive, e.g. metallic pattern
    • H05K1/092—Dispersed materials, e.g. conductive pastes or inks
    • H05K1/095—Dispersed materials, e.g. conductive pastes or inks for polymer thick films, i.e. having a permanent organic polymeric binder

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Abstract

A method for preparing an organic silver solution is provided to allow a rapid/simple production process and to ensure excellent continuous/mass productivity and good quality. A method for preparing an organic silver solution includes a step of reacting an organic material solution containing a carboxylic acid dissolved in alcohol with a silver salt to produce precipitates, followed by dissolving the precipitates in an amine-based solvent. A base of the silver salt is one selected from sodium hydroxide, triethylamine, and dimethylformamide, or a mixture thereof. The carboxylic acid is one selected from formic acid, acetic acid, lauric acid, pivalic acid, and trifluoric acid, or a mixture thereof.

Description

유기은 용액의 제조방법{Synthesis of Organic Silver Solution}Synthesis of Organic Silver Solution

본 발명은 도전성 유기 은 용액의 제조방법에 관한 것으로 보다 상세하게는 전기/전자 회로 구성을 위한 도전성 피막 회로나 전자파 차폐를 위한 박막 등을 구성하거나 금속 분말 등과 혼합한 도전성 페이스트 등을 제조할 때 보다 신속/간단하고 연속/대량 생산이 가능하여 생산성이 우수할 뿐 아니라 친환경적이면서 저렴하고 고품질까지 제공할 수 있는 도전성 유기 은 용액 제조방법에 관한 것이다.The present invention relates to a method for producing a conductive organic silver solution, and more particularly, to prepare a conductive coating circuit for electric / electronic circuit composition, a thin film for electromagnetic shielding, or a conductive paste mixed with metal powder or the like. The present invention relates to a method for preparing a conductive organic silver solution that can provide fast, simple, continuous and mass production, which is excellent in productivity and eco-friendly, inexpensive and high quality.

통상 전기/전자 회로 구성을 위한 도전성 피막회로나 전자파 차폐를 위한 다양한 형태의 전자차폐용 박막 등을 형성할 때 또는 금속 분말 등과 혼합한 도전성 페이스트 등을 제조할 때 에칭법이나 진공증착법 등을 이용하여 형성시키는 것이 일반적인 방법이다.In general, when forming a conductive coating circuit for electric / electronic circuit composition, a thin film for electromagnetic shielding of various forms for electromagnetic shielding, or when manufacturing a conductive paste mixed with metal powder or the like using an etching method or a vacuum deposition method, etc. Forming is a common method.

그런데 상기한 에칭법의 경우는 넓은 면적에 금속 도전막을 만든 후 필요한 부분만 남기고 나머지 부분은 화학적으로 제거하는 방법임에 따라서 막대한 금속재료의 손실이 불가피할 뿐만 아니라 이 과정에서 환경 유해요소인 화학 부산물이 다 량 배출되어 환경오염의 주 원인으로 작용하는 문제점 등이 있다. However, in the case of the etching method, a metal conductive film is formed in a large area, and only the necessary parts are left, and the remaining parts are chemically removed. Therefore, a huge amount of metal material is inevitably lost, and chemical by-products which are environmental hazards in this process are inevitable. There is a problem that a large amount is emitted and acts as a major cause of environmental pollution.

상기 진공증착법 역시도 도금공정 중 환경에 심각한 영향을 주는 폐기물이 다량 발생하는 문제점은 물론 이와 함께 복잡하고 생산 공정 시간이 아주 많이 소요되는 문제점이 있을 뿐 아니라, The vacuum deposition method also has a problem that a large amount of waste that seriously affects the environment during the plating process, as well as a complex and very time-consuming production process,

특히 상기 진공증착법으로 제조할 경우 높은 전기전도성을 가진 막을 제조할 수 있으나, 설비투자액이 커지며 대형화 및 대량생산이 어렵다는 단점이 있다. In particular, when the vacuum deposition method is used to produce a film having a high electrical conductivity, but has a disadvantage in that the investment in equipment is large, and the size and mass production are difficult.

이에 본 발명에서는 상기한 문제점을 일소하기 위해 창안한 것으로서, 먼저 은에 비해 낮은 온도에서 도전성 피막 형성과 환경 및 고정상의 문제들의 해결이 가능하면서도 신속/간단한 제조공정은 물론 뛰어난 연속/대량 생산성과 우수한 품질까지 제공되는 새로운 도전성 물질인 유기은 용액 제조방법을 제공하는 데 주안점을 두고 그 기술적 과제로서 완성한 것이다.Accordingly, the present invention has been devised to eliminate the above problems, first of all, it is possible to solve the problem of the formation of the conductive film and the environmental and fixed phase at a lower temperature than the silver, but also the rapid / simple manufacturing process as well as the excellent continuous / mass productivity and excellent Organic, a new conductive material that provides quality, has been completed as a technical problem with the focus on providing a solution manufacturing method.

위 기술적 과제를 달성하기 위해 본원에서는 아래의 실시예를 통해 보다 구체적으로 살펴보면 하기와 같다.In order to achieve the above technical problem, the present disclosure will be described in more detail through the following examples.

즉, 본 발명은 수화나트륨과 같은 염기의 물질을 증류수에 용해시키고, 여기에 알코올에 용해시킨 카르복실산을 포함하는 유기산 물질을 천천히 첨가해 상온 에서 약10 ~ 60분간 교반해 충분히 반응시킨 다음 이 용액에 질산은을 첨가하면 흰색 침전물의 유기은 화합물이 형성된다. That is, in the present invention, a base material such as sodium hydride is dissolved in distilled water, and an organic acid material including carboxylic acid dissolved in alcohol is slowly added thereto, stirred at room temperature for about 10 to 60 minutes, and then sufficiently reacted. The addition of silver nitrate to the solution results in the formation of organic silver compounds in white precipitates.

이 유기은 화합물은 아주 다양한 용액에서 용해되기는 하지만, 본 발명의 응용목적 중 하나인 도전성 피막형성의 기능성을 감안할 때 아민계의 용매를 이용해 용해하는 것이 바람직하다.Although this organic silver compound is dissolved in a wide variety of solutions, it is preferable to dissolve using an amine solvent in view of the functionality of the conductive film formation, which is one of the application purposes of the present invention.

이를 화학식으로 나타내면 아래 식과 같다.This is represented by the following formula.

Figure 112006031942447-pat00001
Figure 112006031942447-pat00001

이렇게 얻은 상기 유기은 화합물은 분자당 은의 함량이 40~91w%까지 가능하며, 원하는 물질만을 높은 수득율로 손쉽게 얻을 수 있다는 장점을 가지고 있는 것을 알 수 있었다. The organic silver compound thus obtained was found to have an advantage that the content of silver per molecule can be up to 40-91 w%, and only the desired material can be easily obtained at a high yield.

그리고 상기 합성된 유기은 화합물은 아민계 용매 단일 또는 혼합용매에 용해시키고, 침전물을 아민계 용액의 용매로 용해시켜서 된 것 등을 이용해 그 용해속도를 증가 시키기면, If the synthesized organic silver compound is dissolved in a single or mixed solvent of an amine solvent, and the precipitate is dissolved in a solvent of an amine solution to increase its dissolution rate,

은에 비해 낮은 온도에서 도전성 피막 형성과 환경 및 고정상의 문제들의 해 결이 가능하면서도 신속/간단한 제조공정은 물론 뛰어난 연속/대량 생산성이 제공되는 새롭고 우수한 품질의 유기은 용액을 제조할 수 있었다. Compared to silver, it was possible to produce new, high-quality organic silver solutions that provided conductive film formation, solved environmental and stationary problems, while providing fast / simple manufacturing processes as well as excellent continuous / mass productivity.

이하, 각 실시예를 제시한다. Hereinafter, each Example is shown.

<< 실시예Example 1>  1>

실시예 1은 수산화나트륨 2.74g을 증류수에 용해시키고, 에탄올에 용해된 피발릭산 7.00g을 천천히 첨가한 후 약 10분간 상온에서 교반 시킨 다음 증류수에 용해된 질산은 11.6g을 첨가하면 흰색의 침전물이 형성되는데, 이때 얻어진 침전물을 아민계 용매에 용해시켜주면 20%의 연분홍색의 유기은 용액을 얻을 수 있었다. In Example 1, 2.74 g of sodium hydroxide was dissolved in distilled water, 7.00 g of pivalic acid dissolved in ethanol was slowly added, followed by stirring at room temperature for about 10 minutes. Then, 11.6 g of silver nitrate dissolved in distilled water was added to form a white precipitate. When the obtained precipitate was dissolved in an amine solvent, 20% pale pink organic silver solution was obtained.

이렇게 합성/생성된 유기은 용액을 유리표면에 코팅한 다음 180℃에서 1분간 가열하면 고품질의 은 박막을 얻었고, 이은 박막의 비저항은 9x10-6Ω cm으로서 우수한 도전성을 가지고 있다는 것을 알 수 있었다.The synthesized / generated organic silver solution was coated on a glass surface, and then heated at 180 ° C. for 1 minute to obtain a high quality silver thin film. The specific resistance of the silver thin film was 9 × 10 −6 μm cm, indicating that it had excellent conductivity.

<< 실시예Example 2>  2>

실시예 2는 질산은 5.00g을 DMF(다이메틸폼아마이드)에 용해시키고, 트리플루오르산 4.00 g을 첨가하여 상온에서 약 10분간 교반시켜 흰색 침전물을 얻었는데, 이때 얻어진 침전물을 아민계을 포함한 글라이콜 용매에 용해시킨 결과 약 16 %의 무색 유기은 용액을 얻을 수 있었다.In Example 2, 5.00 g of silver nitrate was dissolved in DMF (dimethylformamide), and 4.00 g of trifluoric acid was added thereto, followed by stirring at room temperature for about 10 minutes to obtain a white precipitate. As a result of dissolving in a solvent, a colorless organic silver solution of about 16% was obtained.

이렇게 합성/생성된 유기은 용액을 유리 표면에 코팅한 다음 160℃에서 5분간 가열하여 은 박막을 얻었고, 이때 생산된 은 박막 또한 비저항 6.8x10-5Ω cm으로서 그 도전성이 우수한 것임을 알 수 있었다.The organic silver solution thus synthesized / coated was coated on a glass surface and heated at 160 ° C. for 5 minutes to obtain a silver thin film. The produced silver thin film also has a specific resistance of 6.8 × 10 −5 μm cm, which shows that its conductivity is excellent.

<< 실시예Example 3>  3>

실시예 3은 수산화나트륨 2.32g을 증류수에 용해시키고, 에탄올에 용해된 라울릭산 11.6g을 천천히 첨가한 후 약 10분간 상온에서 교반 시킨 다음 증류수에 용해된 질산은 9.86g을 첨가하면 흰색의 침전물이 형성되는데, 이때 얻어진 침전물을 1차, 2차 아민계 혼합 용매에 용해시켜 은 함량이 17wt%인 투명한 유기은 용액을 얻을 수 있었다.In Example 3, 2.32 g of sodium hydroxide was dissolved in distilled water, 11.6 g of lauric acid dissolved in ethanol was slowly added, stirred at room temperature for about 10 minutes, and 9.86 g of silver nitrate dissolved in distilled water was added to form a white precipitate. In this case, the obtained precipitate was dissolved in a primary and secondary amine mixed solvent to obtain a transparent organic silver solution having a silver content of 17 wt%.

이렇게 합성/생성된 유기은 용액을 유리 표면에 코팅한 다음 200℃에서 10분간 가열하여 은 박막을 얻었고, 이때 얻어진 은 박막의 비저항이 1.9x10-6Ωcm로서 이 또한 우수한 도전성이 있음을 알 수 있었다.The organic silver solution thus synthesized / generated was coated on a glass surface, and then heated at 200 ° C. for 10 minutes to obtain a silver thin film. The specific resistance of the obtained silver thin film was 1.9 × 10 −6 μm cm, which also shows excellent conductivity.

<< 실시예Example 4> 4>

실시예 4는 수산화나트륨 1.80g을 증류수에 용해시키고, 에탄올에 용해된 85% 개미산10.0g을 천천히 첨가한 후 약 10분간 상온에서 교반 시킨 다음 증류수에 용해된 질산은 15.3g을 첨가하면 갈회색의 침전물이 형성되는데, 이때 얻어진 침전 물을 1차, 2차 아민계 용매와 벤젠계 용매의 혼합 용매에 용해시켜 은 함량이 50wt%이상인 짙은 녹색의 고농도 유기 은 용액을 얻었을 수 있었다.In Example 4, 1.80 g of sodium hydroxide was dissolved in distilled water, 10.0 g of 85% formic acid dissolved in ethanol was added slowly, followed by stirring at room temperature for about 10 minutes, and then 15.3 g of silver nitrate dissolved in distilled water was added to the brownish gray precipitate. In this case, the precipitate obtained was dissolved in a mixed solvent of a primary and a secondary amine solvent and a benzene solvent to obtain a dark green high concentration organic silver solution having a silver content of 50 wt% or more.

이렇게 합성/생성된 유기은 용액을 유리 표면에 코팅한 다음 이를 100℃에서 1분간 가열하여 은 박막을 형성시킬 수 있었는데, 이때 얻어진 은 박막의 비저항은 5x10-6Ω cm으로서 우수한 정도성을 가지고 있음을 알 수 있었다.The synthesized / generated organic silver solution was coated on a glass surface and then heated at 100 ° C. for 1 minute to form a silver thin film. The specific resistance of the obtained silver thin film was 5 × 10 −6 Ω cm, indicating that it has excellent accuracy. Could know.

<< 실시예Example 5> 5>

실시예 5는 수산화나트륨 2.32g을 증류수에 용해시키고, 에탄올에 용해된 초산 3.48g을 천천히 첨가한 후 약 10분간 상온에서 교반 시킨 다음 증류수에 용해된 질산은 9.86g을 첨가하면 흰색 침전물이 형성되는 데, 이때 얻어진 침전물을 1차, 2차 아민계 용매와 벤젠계 용매를 혼합한 용매에 용해시켜 은 함량이 25wt%인 투명한 유기은 용액을 얻을 수 있었다.In Example 5, 2.32 g of sodium hydroxide was dissolved in distilled water, 3.48 g of acetic acid dissolved in ethanol was slowly added, stirred at room temperature for about 10 minutes, and 9.86 g of silver nitrate dissolved in distilled water was added to form a white precipitate. The precipitate obtained was dissolved in a solvent in which a primary, secondary amine solvent and a benzene solvent were mixed to obtain a transparent organic silver solution having a silver content of 25 wt%.

이렇게 합성/생성된 유기은 용액을 유리 표면에 코팅한 다음 이를 150℃에서 5분간 가열하면 은 박막을 얻고, 이때 얻어진 은 박막의 비저항은 8x10-6Ω cm으로서 이 또한 우수한 도전성을 나타냄을 알 수 있었다.When the organic silver solution thus synthesized / coated was coated on the glass surface, and then heated at 150 ° C. for 5 minutes, a silver thin film was obtained. The specific resistance of the obtained silver thin film was 8 × 10 −6 Ω cm, which also shows excellent conductivity. .

이상과 같이 살펴본 본 발명의 유기은 용액제조방법은 전술된 바와 같이 우선 은에 비해 낮은 온도에서 도전성 피막(박막 등) 형성이 가능한 유기은 용액을 제조할 때 그 제조설비 및 생산 공정이 아주 간단하고, 보다 저렴한 원가로 연속 대량생산까지 가능함에 따라 우수한 생산성이 제공될 뿐 아니라 특히 도전성 피막 형성시 기존 에칭공정에서의 금속물 손실 등이 전혀 나타나지 않음은 물론 무엇보다 환경 유해요소인 화학 부산물이 전혀 발생되지 않기 때문에 환경오염에 전혀 영향을 주지 않는 친환경성의 효과까지 제공되는 등 그 기대되는 바가 실로 다대한 발명이다.As described above, the organic silver solution manufacturing method of the present invention, as described above, is very simple when manufacturing an organic silver solution that can form a conductive film (thin film, etc.) at a lower temperature than silver, As it is possible to produce continuous mass production at low cost, it not only provides excellent productivity but also does not show any metal loss in the existing etching process, especially when forming a conductive film, and above all, does not generate any chemical by-products that are harmful to the environment. Therefore, the invention is expected to provide an eco-friendly effect that does not affect environmental pollution at all.

Claims (7)

알코올에 용해시킨 카르복실산을 포함하는 유기물 용액에 은염을 반응시켜 침전물을 생성시킨 다음, 그 침전물을 아민계 용액의 용매로 용해시켜 제조하되,A silver salt is reacted with an organic solution containing carboxylic acid dissolved in alcohol to produce a precipitate, and then the precipitate is dissolved in a solvent of an amine solution. 상기 은염의 염기는 수산화나트륨, 트리에틸아민, 다이메틸폼아마이드 중 선택된 하나 또는 하나이상 혼합하여 사용한 것을 특징으로 한 유기은 용액제조방법.The base of the silver salt is an organic silver solution manufacturing method, characterized in that used in one or more selected from sodium hydroxide, triethylamine, dimethylformamide. 제 1항에 있어서,The method of claim 1, 상기 카르복실산은 개미산, 초산, 라울릭산, 피발릭산, 트리플루오르산 중 선택된 하나 또는 하나이상 혼합하여 사용한 것을 특징으로 한 유기은 용액제조방법.The carboxylic acid is a method for producing an organic silver solution, characterized in that used by mixing one or more selected from formic acid, acetic acid, lauric acid, pivalic acid, trifluoric acid. 제 1항에 있어서,The method of claim 1, 상기 아민계 용액의 용매는 1차 또는 2차 아민계 용액 중 하나 또는 하나이상 혼합된 용액을 사용한 것을 특징으로 하는 유기은 용액제조방법.The solvent of the amine-based solution is an organic silver solution manufacturing method, characterized in that using a solution of one or more of the primary or secondary amine-based solution. 제 1항에 있어서,The method of claim 1, 상기 아민계 용액의 용매로 청구항 5의 아민용매에 벤젠계 용매를 더 혼합하여 사용한 것을 특징으로 하는 유기은 용액제조방법.A method for producing an organic silver solution, characterized by further mixing a benzene solvent with the amine solvent of claim 5 as a solvent of the amine solution. 삭제delete 삭제delete 삭제delete
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR0181572B1 (en) * 1995-11-02 1999-04-01 김화중 Method of manufacturing silver powder
JP2003346574A (en) 2002-05-24 2003-12-05 Mitsubishi Paper Mills Ltd Silver salt/amine composite
KR20040084570A (en) * 2003-03-28 2004-10-06 (주)해은켐텍 Organic silver conpound and it's preparation method, organic silver ink and it's direct wiring method
KR100473478B1 (en) 2002-11-20 2005-03-11 (주)나눅스 Silver colloid and preparation method thereof
KR20060028350A (en) * 2004-09-25 2006-03-29 주식회사 잉크테크 Organic silver compounds, organic silver ink and it's direct wiring method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR0181572B1 (en) * 1995-11-02 1999-04-01 김화중 Method of manufacturing silver powder
JP2003346574A (en) 2002-05-24 2003-12-05 Mitsubishi Paper Mills Ltd Silver salt/amine composite
KR100473478B1 (en) 2002-11-20 2005-03-11 (주)나눅스 Silver colloid and preparation method thereof
KR20040084570A (en) * 2003-03-28 2004-10-06 (주)해은켐텍 Organic silver conpound and it's preparation method, organic silver ink and it's direct wiring method
KR20060028350A (en) * 2004-09-25 2006-03-29 주식회사 잉크테크 Organic silver compounds, organic silver ink and it's direct wiring method

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