KR100368055B1 - Synthesis of Spherical Fine Silver Powders at Room Temperature - Google Patents
Synthesis of Spherical Fine Silver Powders at Room Temperature Download PDFInfo
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- KR100368055B1 KR100368055B1 KR10-2000-0050850A KR20000050850A KR100368055B1 KR 100368055 B1 KR100368055 B1 KR 100368055B1 KR 20000050850 A KR20000050850 A KR 20000050850A KR 100368055 B1 KR100368055 B1 KR 100368055B1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
- B22F2009/245—Reduction reaction in an Ionic Liquid [IL]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/25—Noble metals, i.e. Ag Au, Ir, Os, Pd, Pt, Rh, Ru
- B22F2301/255—Silver or gold
Abstract
본 발명은 상온에서 구상형 미립 은 분말의 상온 제조 방법에 관한 것으로, 그 목적은 고온공정을 피하여 에너지 소모를 줄임과 동시에 완전한 구형인 1∼2㎛ 크기의 입도분포가 균질한 은 분말을 제조하는 방법을 제공하는데 있다.본 발명은 1∼2㎛ 크기의 충전제용 구상형 은 분말을 제조하는 방법에 있어서, 질산은 50∼500g/ℓ을 상온에서 증류수에 완전히 용해시키고 암모니아수를 첨가하여 pH를 11로 맞추는 단계와, 다른 용기에 환원제로 사용한 하이드로퀴논을 16.5∼165g/ℓ을 넣고 상온에서 증류수로 완전히 용해시키는 단계와, 상기 두 용액을 반응기에 넣어 혼합 후 상온으로 10∼180분 반응시키는 단계와, 상기 반응이 종료되면 고/액을 분리하고 증류수를 이용해 여러 번 세척한 다음 50℃로 24시간이상 건조하는 단계로 이루어진 것을 특징으로 한다.The present invention relates to a method for producing a spherical fine silver powder at room temperature at room temperature, the purpose of which is to reduce the energy consumption by avoiding the high temperature process and at the same time to produce a homogeneous silver powder with a particle size distribution of 1 ~ 2㎛ size that is completely spherical. The present invention provides a method for producing spherical silver powder for filler having a size of 1 to 2 μm, wherein 50 to 500 g / l of nitric acid is completely dissolved in distilled water at room temperature and ammonia water is added to bring the pH to 11. Matching step, adding 16.5 to 165 g / l of hydroquinone used as a reducing agent in another container and completely dissolving it in distilled water at room temperature; and mixing the two solutions in a reactor and reacting at room temperature for 10 to 180 minutes; When the reaction is completed, the solid / liquid is separated and washed several times with distilled water and then dried at 50 ℃ for 24 hours .
Description
본 발명은 구상형 미립 은 분말의 상온 제조 방법에 관한 것으로, 자세하게는 질산은과 환원제 하이드로퀴논을 상온에서 반응시켜 질산은으로부터 페이스트용 충전제인 구상형 미립 은 분말을 제조하는 기술에 관한 것이다.The present invention relates to a method for producing spherical fine silver powder at room temperature, and more particularly, to a technique for producing spherical fine silver powder which is a filler for paste from silver nitrate by reacting silver nitrate with a reducing agent hydroquinone at normal temperature.
첨단산업과 산업기술의 발달에 따라 고기능성의 정밀소재에 대한 요구가 급증하게 되고, 이에 따라 강도, 경도, 내마모성, 중량 등을 개선하기 위한 고도로 제어된 물리·화학적 특성(입도, 형상, 분산성, 순도, 반응성 등)을 제공할 수 있는 미립의 원료분말(금속, 비금속, 세라믹)이 필요하게 되었다.With the development of high-tech industries and industrial technologies, the demand for high-performance precision materials increases rapidly, and accordingly, highly controlled physical and chemical properties (particle size, shape, dispersibility) to improve strength, hardness, wear resistance, weight, etc. Fine raw material powders (metals, nonmetals, ceramics) capable of providing (purity, reactivity, etc.) have been required.
최근 재료개발동향 중 많은 발전을 이룬 초전도 재료, 비정질 합금, 기계적 합금(mechanical alloying), 나노-합성물 재료 등 우수한 물리적 특성과 기능성이 요구되는 재료에는 대부분 미립분말이 사용되고 있다. 특히 고밀도 집적회로를 채용하고 있는 전자기기의 보급이 급속도로 증가함에 따라 처리능력 향상을 위해 전자회로 소자는 미소화, 고기능화, 다양화 그리고 정밀화되고 있으며 아울러 전자파의 간섭을 방지하기 위한 고정밀의 차폐재료가 요구되고 있다. 이에 따라 고기능성 도전성 페이스트, 전도성 잉크, 전기재료 접착제 등이 전기소자나 전자부품 제조에 필수적으로 사용되고 있다.Recently, fine powders are used for materials requiring excellent physical properties and functionality, such as superconducting materials, amorphous alloys, mechanical alloying, and nano-composite materials, which have made much progress in recent material development trends. In particular, as the spread of electronic devices employing high-density integrated circuits increases rapidly, electronic circuit elements have been miniaturized, highly functionalized, diversified, and precisiond to improve processing capacity, and high-precision shielding materials to prevent electromagnetic interference. Is required. Accordingly, high functional conductive pastes, conductive inks, electrical material adhesives, and the like are essential for the production of electric devices and electronic components.
특히 화학적으로 안정하고 도전성이 우수한 은 페이스트(silver paste)는 전도성 접착, 코팅 그리고 미세회로 형성을 위한 복합계 도전성 페이스트로 널리 사용되고 있으며 앞으로 응용 범위가 더욱 확대될 것으로 예측된다. 현재 국내에서 소비되는 은 페이스트는 대부분 Dupont, Engelhard, Acheson 등으로부터 완제품 상태로 수입하고 있으며 군소업체에서 귀금속 원료분말을 수입하여 유기성 결합제와 단순혼합하여 일부 시판하고 있는 실정이다. 따라서 페이스트용 충전제인 은분말 제조기술의 국산화가 절실히 필요한 시점이다.In particular, chemically stable silver paste has been widely used as a composite conductive paste for conductive adhesion, coating, and microcircuit formation, and is expected to be further expanded in the future. Currently, silver pastes consumed in Korea are mostly imported from Dupont, Engelhard, Acheson, etc. as a finished product, and a small company imports precious metal raw powder and simply mixes it with an organic binder to market it. Therefore, localization of silver powder manufacturing technology, a filler for paste, is urgently needed.
일반적인 은 분말은 화학적 공정 (chemical process), 물리적 공정(physical process) 등을 들 수 있으나 제조방법에 따라 은 분말의 밀도, 표면적, 평균입도,형태 그리고 입도분포 등이 변하게 된다.The general silver powder may include a chemical process and a physical process, but the density, surface area, average particle size, shape, and particle size distribution of the silver powder change depending on the manufacturing method.
은 화합물을 수용액 또는 유기용매에서 환원성 가스나 유기환원제로 환원시켜 은 분말을 석출시키는 화학적 공정에서는 합성한 은 분말의 입자크기가 매우 작고, 입도분포가 좁으며, 순도가 높은 특징이 있다. 최근에는 다양한 종류의 구형 금속분말 제조에 적용할 수 있는 폴리올법이 개발되었으나 반응온도가 150℃ 이상으로 높은 문제점이 있고 환원성 가스로 수소를 사용하는 경우에는 고온·고압반응기(autoclave)를 필요로 하기 때문에 취급시 특별한 주의를 하여야 한다. 물리적 공정은 주로 인편상(flake type)의 은 분말을 제조하는데 사용되지만 미세한 입자를 얻기가 어렵고 입자형태가 불규칙한 단점이 있다.In the chemical process of precipitating silver powder by reducing the silver compound with a reducing gas or an organic reducing agent in an aqueous solution or an organic solvent, the synthesized silver powder has a very small particle size, a narrow particle size distribution, and high purity. Recently, a polyol method has been developed that can be applied to the production of various kinds of spherical metal powder, but the reaction temperature is higher than 150 ℃, and when using hydrogen as a reducing gas, a high temperature autoclave is required. Special care must be taken when handling. The physical process is mainly used to prepare flake type silver powder, but it is difficult to obtain fine particles and has a disadvantage in that the particle shape is irregular.
상기와 같은 문제점을 해결하기 위한 본 발명의 목적은 고온공정을 피하여 에너지 소모를 줄임과 동시에 완전한 구형인 1∼2㎛ 크기의 입도분포가 균질한 은 분말을 제조하는 방법을 제공하는데 있다.상기 본 발명의 목적은 은 페이스트 제조시 충전제로 사용되고 있는 미립의 은분말 제조기술을 확립하고자 하였으며 이를 위하여 하이드로퀴논을 유기환원제로 이용하여 상온에서 구상형 미립 은 분말을 제공함으로써 달성된다.SUMMARY OF THE INVENTION An object of the present invention for solving the above problems is to provide a method of producing a homogeneous silver powder having a homogeneous particle size distribution of 1 to 2 μm while avoiding high temperature processes and reducing energy consumption. An object of the present invention was to establish a fine silver powder manufacturing technology used as a filler in the production of silver paste, and to achieve this, it is achieved by providing a spherical fine silver powder at room temperature using hydroquinone as an organic reducing agent.
도 1 은 실시예 1의 회절분석도1 is a diffractogram of Example 1
도 2 는 실시예 1의 주사 전자 현미경 확대사진2 is a magnified photograph of a scanning electron microscope of Example 1
도 3 은 실시예 2의 회절분석도3 is a diffractogram of Example 2
도 4 는 실시예 2의 주사 전자 현미경 확대사진4 is a magnified photograph of a scanning electron microscope of Example 2
도 5 은 실시예 3의 회절분석도5 is a diffractogram of Example 3
도 6 는 실시예 3의 주사 전자 현미경 확대사진6 is a magnified photograph of a scanning electron microscope of Example 3
이하 본 발명을 상세히 설명하면 다음과 같다.본 발명은 1∼2㎛ 크기의 충전제용 구상형 은 분말을 제조하는 방법에 있어서,질산은 50∼500g/ℓ을 상온에서 증류수에 완전히 용해시키고 암모니아수를 첨가하여 pH를 11로 맞추는 단계와,다른 용기에 환원제로 사용한 하이드로퀴논을 16.5∼165g/ℓ을 넣고 상온에서 증류수로 완전히 용해시키는 단계와,상기 두 용액을 반응기에 넣어 혼합 후 상온으로 10∼180분 반응시키는 단계와,상기 반응이 종료되면 고/액을 분리하고 증류수를 이용해 여러 번 세척한 다음 50℃로 24시간이상 건조하여 은 분말을 제조하는 단계로 이루어진다.상기에서 반응온도를 상온으로 한정한 이유는 은 분말은 상온에서도 제조가 가능하며 온도를 높일 경우 응집현상이 일어날 가능성이 있기 때문이다.질산은의 농도를 한정한 이유는 고액농도가 500g/ℓ보다 큰 조건에서는 은 분말의 회수율이 80%에 불과하여 반응시간이 길어진다는 단점이 있고, 또한 50g/ℓ미만의 조건에서는 98%이상 환원되지만 생산성이 너무 떨어져 제조단가가 높아지는 문제점이 있어 그 구간을 한정하였다.상기 반응시간을 한정한 이유는 10분보다 짧을 경우에는 환원반응이 종료되지 않으며(80% 이하), 반응시간이 180분 보다 길 경우에는 은 분말의 입자크기가 불균일해진다는 단점이 있기 때문이다.상기 하이드로퀴논의 첨가량을 한정한 이유는 하이드로퀴논에 의한 질산은의 반응시 하이드로퀴논 1분자에서 2개의 전자가 나오므로 은 이온 2몰을 하이드로퀴논으로 환원이 가능하다. 여기서 하이드로 퀴논의 첨가량은 몰비 0.5를 고려한 수치이며 이보다 적은 양이 첨가되면 은 분말의 회수율이 떨어지게 된다.Hereinafter, the present invention will be described in detail. The present invention provides a method for producing spherical silver powder for filler having a size of 1 to 2 μm, wherein 50 to 500 g / L of nitric acid is completely dissolved in distilled water at room temperature and ammonia water is added. Adjusting the pH to 11, adding 16.5 to 165 g / l of hydroquinone used as a reducing agent in another vessel and completely dissolving it in distilled water at room temperature, and mixing the two solutions in a reactor for 10 to 180 minutes at room temperature. Reacting step, and when the reaction is complete, separating the solid / liquid, and washed several times with distilled water and then dried at 50 ℃ for 24 hours or more to produce a silver powder. The reason is that silver powder can be manufactured at room temperature and coagulation may occur if the temperature is increased. Under the condition that the concentration is higher than 500g / ℓ, the recovery time of silver powder is only 80% and the reaction time is long. Also, under the conditions of 50g / ℓ, it is reduced by more than 98%, but the productivity is so low that the manufacturing cost increases. The reason for limiting the reaction time is that when the reaction time is shorter than 10 minutes, the reduction reaction does not end (80% or less), and when the reaction time is longer than 180 minutes, the particle size of the silver powder is uneven. The reason for limiting the addition amount of the hydroquinone is that two electrons are emitted from one molecule of hydroquinone during the reaction of the silver nitrate by the hydroquinone, so that two moles of silver ions can be reduced to hydroquinone. Here, the amount of hydroquinone added is a value considering a molar ratio of 0.5, and when a smaller amount is added, the recovery rate of silver powder is reduced.
본 발명에 따른 실시예를 설명하면 다음과 같다.본 발명에서는 국내산 질산은을 원료로, 환원제로는 하이드로퀴논(Junsei, 일본)을 사용하였으며, 반응온도는 상온, 실험장치로는 테플론 재질의 비이커를 사용하였다.An embodiment according to the present invention will be described as follows. In the present invention, domestic silver nitrate is used as a raw material, and a hydroquinone (Junsei, Japan) is used as a reducing agent. Used.
<실시예 1><Example 1>
질산은 50g을 500㎖의 증류수에 완전히 용해시킨 후 마그네틱바로 교반시키면서 pH가 11이 되도록 암모니아수를 첨가한다. 하이드로퀴논 16.5g을 500㎖의 증류수에 완전히 용해시킨다. 각각의 용액을 테플론 비이커에 혼합한다. 혼합 후 10분이 지나면 여과하여 고/액 분리한다. 증류수로 수회 세척하고 전기오븐에서 50℃로 24시간이상 건조한다. 건조된 은 분말은 X-선 회절분석기와 주사전자현미경을 통해 확인하였다.50 g of silver nitrate is completely dissolved in 500 ml of distilled water, and ammonia water is added so that the pH is 11 while stirring with a magnetic bar. 16.5 g of hydroquinone are completely dissolved in 500 ml of distilled water. Each solution is mixed in a Teflon beaker. After 10 minutes of mixing, the solution is separated by filtration. Wash several times with distilled water and dry at 50 ℃ for more than 24 hours in electric oven. The dried silver powder was confirmed by X-ray diffractometer and scanning electron microscope.
<실시예 2><Example 2>
질산은 50g을 500㎖의 증류수에 완전히 용해시키고 마그네틱바로 교반시키면서 pH가 11이 되도록 암모니아수를 첨가한다. 하이드로퀴논 16.5g을 500㎖의 증류수에 완전히 용해시킨다. 각각의 용액을 테플론 비이커에 혼합한다. 혼합 후 3시간이 지나면 여과하여 고/액 분리한다. 증류수로 수회 세척하고 전기오븐에서 50℃로 24시간이상 건조한다. 건조된 은 분말은 X-선 회절분석기와 주사전자현미경을 통해 확인하였다.50 g of silver nitrate is completely dissolved in 500 ml of distilled water, and ammonia water is added so that the pH is 11 while stirring with a magnetic bar. 16.5 g of hydroquinone are completely dissolved in 500 ml of distilled water. Each solution is mixed in a Teflon beaker. After 3 hours of mixing, the mixture is filtered to separate solid and liquid. Wash several times with distilled water and dry at 50 ℃ for more than 24 hours in electric oven. The dried silver powder was confirmed by X-ray diffractometer and scanning electron microscope.
<실시예 3><Example 3>
질산은 500g을 500㎖의 증류수에 완전히 용해시키고 마그네틱바로 교반시키면서 pH가 11이 되도록 암모니아수를 첨가한다. 하이드로퀴논 165g을 500㎖의 증류수에 완전히 용해시킨다. 각각의 용액을 테플론 비이커에 혼합한다. 혼합 후 3시간이 지나면 여과하여 고/액 분리한다. 증류수로 수회 세척하고 전기오븐에서 50℃로 24시간이상 건조한다. 건조된 은 분말은 X-선 회절분석기와 주사전자현미경을 통해 확인하였다.본 발명은 상술한 특정의 바람직한 실시예에 한정되지 아니하며, 청구범위에서 청구하는 본 발명의 요지를 벗어남이 없이 당해 발명이 속하는 기술분야에서 통상의 지식을 가진 자라면 누구든지 다양한 변형실시가 가능한 것은 물론이고, 그와 같은 변경은 청구범위 기재의 범위 내에 있게 된다.500 g of silver nitrate is completely dissolved in 500 ml of distilled water and ammonia water is added so that the pH is 11 while stirring with a magnetic bar. 165 g of hydroquinone is completely dissolved in 500 ml of distilled water. Each solution is mixed in a Teflon beaker. After 3 hours of mixing, the mixture is filtered to separate solid and liquid. Wash several times with distilled water and dry at 50 ℃ for more than 24 hours in electric oven. The dried silver powder was identified through an X-ray diffractometer and a scanning electron microscope. The present invention is not limited to the specific preferred embodiments described above, and the present invention is made without departing from the gist of the invention as claimed in the claims. Various modifications can be made by those skilled in the art, and such changes are within the scope of the claims.
본 발명은 질산은을 하이드로퀴논으로 환원시켜 구상형의 미립 은 분말(1∼2㎛)을 제조하는 기술로 상온에서 단시간내에 구상형 미립 은 분말을 제조할 수 있는 기술이다. 때문에 첨단 전자산업의 발달과 더불어 미립 금속분말의 수요가 증대되는 시점과 대부분의 금속분말을 수입에 전량 의존하는 현실에서 본 발명은 수입대체효과 및 공정의 단순화 등에 의해 경제성이 확보되는 효과가 있다.The present invention is a technique for producing spherical fine silver powder (1 ~ 2㎛) by reducing silver nitrate with hydroquinone is a technique that can produce spherical fine silver powder in a short time at room temperature. Therefore, the present invention has the effect of securing economic feasibility due to the import substitution effect and the simplification of the process in the reality that the demand for fine metal powder increases with the development of advanced electronic industry and most of the metal powder is completely dependent on import.
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| KR100954425B1 (en) | 2007-11-02 | 2010-04-26 | 주식회사 지오션 | Method for preparation of silver powder by continuous solution reduction |
| KR20180083226A (en) | 2017-01-12 | 2018-07-20 | 주식회사 테라메탈 | Method of preparing silver powder by continuous solution reduction and the apparatus thereof |
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| KR100610816B1 (en) * | 2004-08-02 | 2006-08-10 | 한국지질자원연구원 | Manufacturing method of silver powder |
| KR100713662B1 (en) * | 2005-10-20 | 2007-05-02 | 한국지질자원연구원 | Manufacturing Process of Sphere Shape Silver Powder from Silver Scrap |
| KR102033545B1 (en) | 2017-06-05 | 2019-10-17 | 대주전자재료 주식회사 | Silver particle and method of manufacture thereof |
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| KR100954425B1 (en) | 2007-11-02 | 2010-04-26 | 주식회사 지오션 | Method for preparation of silver powder by continuous solution reduction |
| KR20180083226A (en) | 2017-01-12 | 2018-07-20 | 주식회사 테라메탈 | Method of preparing silver powder by continuous solution reduction and the apparatus thereof |
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