KR20020017489A - Synthesis of fine cobalt powders - Google Patents

Synthesis of fine cobalt powders Download PDF

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KR20020017489A
KR20020017489A KR1020000050849A KR20000050849A KR20020017489A KR 20020017489 A KR20020017489 A KR 20020017489A KR 1020000050849 A KR1020000050849 A KR 1020000050849A KR 20000050849 A KR20000050849 A KR 20000050849A KR 20020017489 A KR20020017489 A KR 20020017489A
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solution
cobalt powder
fine cobalt
powder
temperature
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KR100368054B1 (en
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김동진
정헌생
이자현
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곽영훈
한국지질자원연구원
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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
    • 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]
    • 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
    • B22F2201/00—Treatment under specific atmosphere
    • B22F2201/01—Reducing atmosphere
    • B22F2201/013—Hydrogen
    • 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
    • B22F2301/15—Nickel or cobalt

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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

PURPOSE: A method for manufacturing fine cobalt powder is provided which combines merits of pressurized hydrogen reduction and polyol methods in order to establish technology for manufacturing sub-micron sized cobalt powder at a relatively low reaction temperature within a short reaction time. CONSTITUTION: The method for manufacturing fine cobalt powder comprises the processes of mixing the resulting materials by adding various additives including PdCl2, PVP and NaOH to the solution after dissolving a certain amount of Co(OH)2 having a concentration of 31 to 95 g/L that is used as a material for manufacturing fine cobalt powder into ethylene glycol that is used as a solvent using a magnetic bar; heating the solution to a reaction temperature of 140 deg.C or more for a reaction time of 10 to 30 minutes as stirring after putting the prepared solution into a high temperature high pressure reactor; charging a certain amount of hydrogen gas into the reactor when the solution heated reaches to a certain set temperature; cooling the solution with cooling water when reduction is terminated, and solid/liquid separating the cooled resulting solution; and obtaining fine cobalt powder by drying the resulting material at 50 deg.C for 24 hours or more after washing the recovered metallic powder several times using ethanol.

Description

미립 코발트 분말의 제조 방법{Synthesis of fine cobalt powders}Synthesis of fine cobalt powders

본 발명은 미립 코발트 분말 제조 방법에 관한 것으로서, 더욱 상세하게는 폴리올법에 의한 코발트 분말 제조시 2시간 이상의 반응시간과 210℃의 반응온도가 필요한 것을 폴리올법과 가압수소환원법을 혼합하여 낮은 온도와 짧은 반응시간에 0.1 ∼ 0.2㎛ 크기의 코발트 분말을 제조하는 방법에 관한 것이다.The present invention relates to a method for preparing fine cobalt powder, and more specifically, a reaction time of 2 hours or more and a reaction temperature of 210 ° C. is required in the preparation of cobalt powder by the polyol method. It relates to a method for producing a cobalt powder of 0.1 to 0.2㎛ size in the reaction time.

첨단산업과 관련기술의 발달에 따라 고기능성의 정밀소재에 대한 요구가 급증하고 있으며, 이에 따라 강도, 경도, 내마모성, 내식성, 내열성 등을 개선하기 위하여 고도로 제어된 물리ㆍ화학적 특성(입도, 형상, 분산성, 순도, 반응성 등)을 보유하고 있는 미립 원료분말의 원활한 공급이 필요한 시점이다.With the development of high-tech industries and related technologies, the demand for high-performance precision materials is increasing rapidly. Therefore, highly controlled physical and chemical properties (particle size, shape, shape, etc.) are improved to improve strength, hardness, wear resistance, corrosion resistance, and heat resistance. It is time to smoothly supply fine raw material powder with dispersibility, purity, and reactivity.

특히 최근의 재료개발 동향 중 많은 발전을 이룬 초전도 재료, 비정질 합금, 기계적 합금(mechanical alloying), 나노-합성물(nano-composite) 재료 등 우수한 물성과 기능성이 요구되는 재료에는 대부분 미립분말이 사용되고 있으며 전자공업의 발전에 따라 전도성 잉크, 페이스트(paste) 그리고 전기재료 접착제의 원료로서 사용되는 서브마이크론 또는 마이크론 크기의 금속분말에 대한 수요가 급증하고 있다.Particularly, 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 many advancements in recent material development trends. As the industry develops, the demand for submicron or micron-sized metal powders used as raw materials for conductive inks, pastes and electrical material adhesives is increasing rapidly.

본 발명에서 개발하고자한 미립의 코발트 분말은 현재 절삭공구, 초합금, 고속도강, 착색제, 레디얼 타이어에서 스틸벨트와 고무사이의 접착제, 그리고 충전용 밧데리의 주요 성분 등으로 널리 사용되고 있다. 특히 텅스텐 카바이드의 경도와 코발트의 연성을 결합하여 우수한 절삭능을 부여한 소결제품의 특성은 코발트 함량과 입자크기에 주로 의존하기 때문에 균질한 형태, 좁은 입도분포 그리고 고순도인 코발트 분말을 경제적인 방법으로 제조하기 위한 연구가 활발히 수행되고 있다.The fine cobalt powder to be developed in the present invention is widely used as cutting tool, super alloy, high speed steel, colorant, adhesive between steel belt and rubber in radial tire, and main component of rechargeable battery. In particular, the characteristics of the sintered product, which combines the hardness of tungsten carbide with the ductility of cobalt and gives excellent cutting ability, are mainly dependent on the cobalt content and particle size. Research to do this is being actively conducted.

코발트 분말은 현재 산화물의 가스에 의한 고온환원법, 유기용매를 이용한 폴리올법, 유기염의 열분해법, 가압수소환원법 등으로 제조하고 있으며 초합금의 고온특성, 고속도 공구강과 소결탄화물의 절삭성, 그리고 고강도강의 인성을 향상시키는데 필수적인 원소이기 때문에 고가임에도 불구하고 분말야금분야에서 사용량이 지속적으로 급증하고 있다.Cobalt powder is currently manufactured by high temperature reduction method using oxide gas, polyol method using organic solvent, pyrolysis method of organic salt, pressurized hydrogen reduction method, etc. Although it is expensive because it is an essential element to improve, the use of powder metallurgy is continuously increasing.

일반적으로, 가압수소환원법에 의하여 코발트 분말 제조시 반응온도는 210℃, 반응시간 30 ∼ 60분이 필요하며 반응산물인 코발트 분말은 응집되는 현상이 있고 코발트 분말의 형상제어가 어려운 단점이 있다.In general, the reaction temperature is 210 ℃, the reaction time 30 ~ 60 minutes is required when the cobalt powder is produced by the pressurized hydrogen reduction method, the cobalt powder is a reaction product is agglomeration phenomenon and the shape control of the cobalt powder is difficult.

또한, 폴리올법은 응집되지 않고 잘 분산된 코발트 분말을 얻을 수 있으나 210℃에서 2시간 이상의 반응이 필요하며 코발트 산화물의 가스에 의한 고온환원법은 불순물이 다량 포함되는 문제점을 갖고 있다.In addition, the polyol method is capable of obtaining cobalt powder that is not aggregated and well dispersed, but requires a reaction of at least 2 hours at 210 ° C., and a high temperature reduction method using a gas of cobalt oxide has a problem of containing a large amount of impurities.

본 발명은 상기한 문제점을 해결하기 위하여 안출한 것으로서, 그 목적은 비교적 낮은 반응온도와 짧은 반응시간내에 서브마이크론 크기의 코발트 분말 제조 기술을 확립하기 위하여 가압수소환원법과 폴리올법의 장점을 혼합한 미립 코발트 분말의 제조 방법을 제공하는 것이다.The present invention has been made to solve the above problems, the object of which is to combine the advantages of the hydrogen reduction method and polyol method in order to establish a submicron size cobalt powder production technology within a relatively low reaction temperature and short reaction time It is to provide a method for producing cobalt powder.

상기한 목적을 달성하기 위하여 본 발명에서는 Co(OH)2(Aldrich, 미국)를 원료로, 용매로는 에틸렌 글리콜(ethylene glycol)(Junsei, 일본)을 사용하였으며, 실험장치로는 고온고압 반응기(autoclave)를 사용하였다.In order to achieve the above object, in the present invention, Co (OH) 2 (Aldrich, USA) was used as a raw material, ethylene glycol (ethylene glycol) (Junsei, Japan) was used as a solvent, and a high temperature high pressure reactor ( autoclave) was used.

도 1 은 본 발명의 실시예 1을 나타낸 회절분석도1 is a diffractogram showing Example 1 of the present invention

도 2 는 본 발명의 실시예 2를 나타낸 회절분석도2 is a diffractogram showing Example 2 of the present invention.

도 3 은 실시예 2를 주사전자현미경으로 본 확대사진Figure 3 is an enlarged photograph of Example 2 seen with a scanning electron microscope

도 4 는 본 발명의 실시예 3을 나타낸 회절분석도4 is a diffractogram showing Example 3 of the present invention.

이하, 본 발명을 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail.

폴리올법과 가압수소환원법을 함께 적용시켜 Co(OH)2로부터 서브마이크론 크기의 코발트 분말을 제조하는 기술에 있어서, 고액농도 31 ∼ 95g/ℓ, 반응온도 140℃ 이상, 반응시간을 10 ∼ 30분으로 한다.In the technique for producing a submicron-sized cobalt powder from Co (OH) 2 by applying the polyol method and the pressurized hydrogen reduction method together, the solid solution concentration of 31 ~ 95g / L, the reaction temperature of 140 ℃ or more, the reaction time to 10 to 30 minutes do.

우선 미립 코발트 분말 제조의 원료로 사용된 Co(OH)2일정량을 용매로 사용한 에틸렌 글리콜(ethylene glycol)에 마그네틱바를 이용하여 용해시키고 각종 첨가제(PdCl2, PVP, NaOH)를 첨가하여 혼합한다. 고온고압 반응기에 준비된 용액을 넣고 교반시키며 가열한다. 설정한 온도에 도달하면 일정량의 수소가스를 장입한다. 환원반응이 종료되면 냉각수로 냉각하고 고/액 분리를 실시한다. 회수된 금속분말은 에탄올을 이용하여 수 회 세척하고 50℃로 24시간 이상 건조하여 미립의 코발트 분말을 얻었다.First, a certain amount of Co (OH) 2 used as a raw material for the preparation of fine cobalt powder is dissolved in ethylene glycol, which is used as a solvent, using a magnetic bar, and various additives (PdCl 2 , PVP, NaOH) are added and mixed. The prepared solution is put into a high temperature and high pressure reactor and heated with stirring. When the set temperature is reached, a certain amount of hydrogen gas is charged. When the reduction reaction is completed, it is cooled with cooling water and solid / liquid separation is performed. The recovered metal powder was washed several times with ethanol and dried at 50 ° C. for at least 24 hours to obtain fine cobalt powder.

본 발명에 따른 실시예를 설명하겠다.An embodiment according to the present invention will be described.

실시예 1Example 1

우선 미립 코발트 분말 제조의 원료로 사용된 Co(OH)215.8g을 상온에서 용매로 사용한 에틸렌 글리콜(ethylene glycol) 300㎖에 용해시키고 에틸렌 글리콜 200㎖에 0.2g의 NaOH를 용해시킨다. NaOH를 용해시킨 용액에 PdCl21㎖와 PVP 5g을 용해시킨다. 각종 첨가제를 용해시킨 용액과 Co(OH)2용액을 교반하면서 혼합한다. 고온고압 반응기에 준비된 용액을 넣고 800rpm으로 교반시키며 140℃까지 가열한다.First, 15.8 g of Co (OH) 2 used as a raw material for preparing cobalt powder was dissolved in 300 ml of ethylene glycol used as a solvent at room temperature, and 0.2 g of NaOH was dissolved in 200 ml of ethylene glycol. 1 ml of PdCl 2 and 5 g of PVP are dissolved in a solution of NaOH. The solution in which the various additives are dissolved and the Co (OH) 2 solution are mixed while stirring. The prepared solution is placed in a high temperature and high pressure reactor, and the mixture is stirred at 800 rpm and heated to 140 ° C.

상기, 설정온도에 도달하면 수소가스를 500psi까지 넣어준다. 30분이 경과하면 반응을 종료하고 냉각수로 냉각시킨 후 반응물을 여과하여 고/액 분리하고 회수된 분말은 에탄올을 이용하여 수 회 세척한다. 전기오븐에서 50℃로 24시간 이상 건조하고, 건조된 코발트 분말은 X-선 회절분석기(XRD)를 이용하여 확인하였다.When the set temperature is reached, hydrogen gas is added up to 500 psi. After 30 minutes, the reaction was terminated, cooled with cooling water, and the reactants were filtered and separated into solid and liquid, and the recovered powder was washed several times with ethanol. After drying at 50 ° C or more in an electric oven for 24 hours, the dried cobalt powder was confirmed using an X-ray diffractometer (XRD).

실시예 2Example 2

미립 코발트 분말 제조의 원료로 사용된 Co(OH)215.8g을 상온에서 용매로 사용한 에틸렌 글리콜 300㎖에 용해시키고 에틸렌 글리콜 200㎖에 0.2g의 NaOH를 용해시킨다. NaOH를 용해시킨 용액에 PdCl21㎖와 PVP 5g을 용해시킨다. 각종 첨가제를 용해시킨 용액과 Co(OH)2용액을 교반하면서 혼합한다. 고온고압 반응기에 준비된 용액을 넣고 800rpm으로 교반시키며 150℃까지 가열한다.15.8 g of Co (OH) 2 used as a raw material for preparing cobalt powder was dissolved in 300 ml of ethylene glycol used as a solvent at room temperature, and 0.2 g of NaOH was dissolved in 200 ml of ethylene glycol. 1 ml of PdCl 2 and 5 g of PVP are dissolved in a solution of NaOH. The solution in which the various additives are dissolved and the Co (OH) 2 solution are mixed while stirring. The prepared solution is placed in a high temperature and high pressure reactor, and the mixture is stirred at 800 rpm and heated to 150 ° C.

상기, 설정 온도에 도달하면 수소가스를 500psi까지 넣어준다. 10분이 경과하면 반응을 종료하고 냉각수로 냉각시킨 후 반응물을 여과하여 고/액 분리하고 회수된 분말은 에탄올을 이용하여 수 회 세척한다. 전기오븐에서 50℃로 24시간 이상 건조하고, 건조된 코발트 분말은 X-선 회절분석기(XRD)와 주사전자현미경(SEM)을 이용하여 확인하였다.When the set temperature is reached, hydrogen gas is added up to 500 psi. After 10 minutes, the reaction was terminated, cooled with cooling water, the reaction product was filtered and separated into solid and liquid, and the recovered powder was washed several times with ethanol. After drying for 24 hours at 50 ℃ in an electric oven, the dried cobalt powder was confirmed by using an X-ray diffractometer (XRD) and a scanning electron microscope (SEM).

실시예 3Example 3

미립 코발트 분말 제조의 원료로 사용된 Co(OH)247.4g을 상온에서 용매로 사용한 에틸렌 글리콜 300㎖에 용해시키고 에틸렌 글리콜 200㎖에 0.2g의 NaOH를용해시킨다. NaOH를 용해시킨 용액에 PdCl21㎖와 PVP 5g을 용해시킨다. 각종 첨가제를 용해시킨 용액과 Co(OH)2용액을 교반하면서 혼합한다. 고온고압 반응기에 준비된 용액을 넣고 800rpm으로 교반시키며 150℃까지 가열한다. 설정온도에 도달하면 수소가스를 500psi까지 넣어준다. 30분이 경과하면 반응을 종료하고 냉각수로 냉각시킨 후 반응물을 여과하여 고/액 분리하고 회수된 분말은 에탄올을 이용하여 수 회 세척한다. 전기오븐에서 50℃로 24시간 이상 건조하고 건조된 코발트 분말은 X-선 회절분석기(XRD)를 이용하여 확인하였다.47.4 g of Co (OH) 2 used as a raw material for the preparation of fine cobalt powder is dissolved in 300 ml of ethylene glycol used as a solvent at room temperature, and 0.2 g of NaOH is dissolved in 200 ml of ethylene glycol. 1 ml of PdCl 2 and 5 g of PVP are dissolved in a solution of NaOH. The solution in which the various additives are dissolved and the Co (OH) 2 solution are mixed while stirring. The prepared solution is placed in a high temperature and high pressure reactor, and the mixture is stirred at 800 rpm and heated to 150 ° C. When the set temperature is reached, add hydrogen gas to 500 psi. After 30 minutes, the reaction was terminated, cooled with cooling water, and the reactants were filtered and separated into solid and liquid, and the recovered powder was washed several times with ethanol. Cobalt powder dried at 50 ° C. or more in an electric oven for 24 hours and dried was identified using an X-ray diffractometer (XRD).

본 발명은 Co(OH)2를 폴리올과 수소가스로 환원시켜 미립의 코발트 분말을 제조하는 기술로 기존의 반응온도보다 50℃ 이상 낮은 온도에서 제조할 수 있고, 반응시간 또한 기존에는 2시간 이상의 반응시간을 필요로 했으나 본 발명에서는 30분 이하로 단시간에 반응이 종료되었다. 이와 같은 발명으로 금속분말의 제조시 반응온도를 낮추고 반응시간을 단축함으로써 에너지를 절약할 수 있는 새로운 공정 개발이 가능한 매우 유용한 발명인 것이다.The present invention is a technology for producing fine cobalt powder by reducing Co (OH) 2 with polyol and hydrogen gas, can be prepared at a temperature lower than 50 ℃ than the conventional reaction temperature, the reaction time is also conventionally 2 hours or more reaction Although time was required, in the present invention, the reaction was terminated in less than 30 minutes. This invention is a very useful invention that can develop a new process that can save energy by lowering the reaction temperature and shortening the reaction time in the production of metal powder.

(변형예, 응용예, 법적해석)(Variants, applications, legal interpretations)

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.The present invention is not limited to the above-described specific preferred embodiments, and various modifications can be made by any person having ordinary skill in the art without departing from the gist of the present invention claimed in the claims. Of course, such changes will fall within the scope of the claims.

Claims (1)

폴리올법과 가압수소환원법을 함께 적용시켜 Co(OH)2로부터 서브마이크론 크기의 코발트 분말을 제조하는 기술로 고액농도 31 ∼ 95g/ℓ, 반응온도 140℃ 이상, 반응시간 10 ∼ 30분으로 부여하는 것을 특징으로 하는 미립 코발트 분말의 제조 방법.Polyol method and pressurized hydrogen reduction method are applied together to produce a submicron size cobalt powder from Co (OH) 2, which gives solid solution concentration of 31-95g / l, reaction temperature of 140 ℃ or more and reaction time of 10-30 minutes. A method for producing particulate cobalt powder, characterized by the above-mentioned.
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KR101353344B1 (en) * 2011-12-05 2014-02-17 한국지질자원연구원 Method for manufacturing cobalt powder using platinum group catalysts and cobalt powder manufactured through the same
CN106964784A (en) * 2017-05-27 2017-07-21 湘潭大学 A kind of preparation method of cobalt powder
KR20200061480A (en) * 2018-11-23 2020-06-03 신라대학교 산학협력단 Method of manufacturing porous metal ball and metal balls produced therefrom

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KR100426824B1 (en) * 2001-09-03 2004-04-14 한국지질자원연구원 Preparation of mono-dispersed fine cobalt powder
KR101252058B1 (en) * 2011-02-10 2013-04-12 한국지질자원연구원 METHOD OF MANUFACTURING Co POWDER USING SLURRY REDUCTION METHOD WITH EXCELLENT DISPERSIVE PROPERTY
KR101252057B1 (en) 2011-02-10 2013-04-12 한국지질자원연구원 METHOD OF MANUFACTURING Co POWDER USING SLURRY REDUCTION METHOD WITH EXCELLENT REACTION VELOCITY
KR101252059B1 (en) * 2011-02-10 2013-04-12 한국지질자원연구원 Apparatus for manufacturing cobalt powder using slurry re reduction method and manufacturing method of manufacturing cupper powder using the same

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Publication number Priority date Publication date Assignee Title
KR101353344B1 (en) * 2011-12-05 2014-02-17 한국지질자원연구원 Method for manufacturing cobalt powder using platinum group catalysts and cobalt powder manufactured through the same
CN106964784A (en) * 2017-05-27 2017-07-21 湘潭大学 A kind of preparation method of cobalt powder
CN106964784B (en) * 2017-05-27 2020-12-08 湘潭大学 Preparation method of cobalt powder
KR20200061480A (en) * 2018-11-23 2020-06-03 신라대학교 산학협력단 Method of manufacturing porous metal ball and metal balls produced therefrom

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