KR20100010076A - Porous nickel metal powders and method for manufacturing same - Google Patents

Porous nickel metal powders and method for manufacturing same Download PDF

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KR20100010076A
KR20100010076A KR1020080070910A KR20080070910A KR20100010076A KR 20100010076 A KR20100010076 A KR 20100010076A KR 1020080070910 A KR1020080070910 A KR 1020080070910A KR 20080070910 A KR20080070910 A KR 20080070910A KR 20100010076 A KR20100010076 A KR 20100010076A
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nickel
metal powder
solution
nickel metal
porous
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KR101051660B1 (en
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최준환
김용진
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한국기계연구원
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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
    • B22F1/14—Treatment of metallic powder
    • 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
    • B22F1/062—Fibrous particles
    • 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
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/15—Nickel or cobalt

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)

Abstract

PURPOSE: Porous nickel metal powder, and a manufacturing method thereof are provided to increase air porosity of the powder by including a reticulate particle structure. CONSTITUTION: A method of porous nickel metal powder is as follows: First solution and second solution formed by selectively mixing polyol, a reducing agent, nickel compound, and polymer additive(S100) are prepared. Mixed solution is formed by adding the first solution to the second solution(S200). Nickel metal powder is created by heating the mixed solution with a uniform temperature(S300). The created nickel metal powder is divided(S400). The divided nickel metal powder is washed and dried(S500).

Description

다공성 니켈 금속분말 및 이의 제조방법 {Porous nickel metal powders and method for manufacturing same }Porous nickel metal powders and method for manufacturing same

도 1 은 본 발명에 의한 다공성 니켈 금속분말의 제조방법을 나타낸 제조공정도.1 is a manufacturing process diagram showing a method for producing a porous nickel metal powder according to the present invention.

도 2 는 본 발명의 제1실시예에 따라 제조된 다공성 니켈 금속분말의 주사전자현미경 사진.2 is a scanning electron micrograph of a porous nickel metal powder prepared according to the first embodiment of the present invention.

도 3 은 본 발명의 제1실시예 및 제2실시예에 따라 제조된 다공성 니켈 금속분말의 기공도 변화를 보인 그래프.Figure 3 is a graph showing the porosity change of the porous nickel metal powder prepared according to the first and second embodiments of the present invention.

도 4 는 본 발명의 제3실시예에 따라 제조된 다공성 니켈 금속분말의 주사전자현미경 사진.Figure 4 is a scanning electron micrograph of the porous nickel metal powder prepared according to the third embodiment of the present invention.

도 5 는 본 발명의 제4실시예에 따라 제조된 다공성 니켈 금속분말의 주사전자현미경 사진.5 is a scanning electron micrograph of the porous nickel metal powder prepared according to the fourth embodiment of the present invention.

도 6 은 본 발명의 제5실시예에 따라 제조된 다공성 니켈 금속분말의 주사전자현미경 사진.6 is a scanning electron micrograph of the porous nickel metal powder prepared according to the fifth embodiment of the present invention.

도 7 은 본 발명에 의한 다공성 니켈 금속분말에 대한 제1비교예의 주사전자현미경 사진.7 is a scanning electron micrograph of the first comparative example for the porous nickel metal powder according to the present invention.

도 8 은 본 발명에 의한 다공성 니켈 금속분말에 대한 제2비교예의 주사전자 현미경 사진.8 is a scanning electron micrograph of a second comparative example for the porous nickel metal powder according to the present invention.

* 도면의 주요 부분에 대한 부호의 설명 *Explanation of symbols on the main parts of the drawings

S100. 재료준비단계 S120. 제1용액준비과정S100. Material preparation step S120. First Solution Preparation Process

S140. 제2용액준비과정 S200. 용액혼합단계S140. Second solution preparation process S200. Solution mixing step

S300. 니켈금속분말생성단계 S400. 니켈금속분말분리단계S300. Nickel metal powder production step S400. Nickel Metal Powder Separation Step

S500. 니켈금속분말세척/건조단계S500. Nickel Metal Powder Cleaning / Drying Step

본 발명은 다공성 니켈 금속분말 및 이의 제조방법에 관한 것으로, 보다 상세하게는 습식법을 통해 제조하여 망목상의 입자구조를 가짐으로써 분말 내부 기공도가 증가하며, 투자비와 공정 비용이 감소하는 이점이 있다.The present invention relates to a porous nickel metal powder and a method of manufacturing the same, and more particularly, by the wet method, having a mesh-like particle structure increases the porosity of the powder, and has the advantage of reducing investment cost and process cost.

니켈 금속분말은 사용되는 분야에 따라 요구되는 특성(입도, 기공도, 표면 특성 등)이 다르게 된다. MLCC (multi-layer ceramic capacitor)용 전극재료로 사용되는 니켈 금속분말은 균일하고 미세한 구형의 입자가 요구되는 반면 연료전지 특히 MCFC (molten carbonate fuel cell)전극, 2차전지용 전극, 촉매 소재 및 전도성폴리머용 충진제에 사용되는 니켈 금속분말은 높은 기공도를 요구하게 된다.Nickel metal powders require different properties (particle size, porosity, surface properties, etc.) depending on the field of use. Nickel metal powders used as electrode materials for MLCC (multi-layer ceramic capacitors) require uniform and fine spherical particles, while fuel cells, especially MCFC (molten carbonate fuel cell) electrodes, secondary battery electrodes, catalyst materials and conductive polymers Nickel metal powders used in fillers require high porosity.

그리고, 종래의 니켈 금속분말을 제조하는 방법으로는 기상법과 액상법이 있다. 기상법은 니켈전구체를 기화시켜 이를 환원, 석출하는 방법으로 분말의 불순물 제어가 상대적으로 용이하지만 제조비용이 높고 생산성이 낮으며 입경제어가 용이 하지 않다는 단점이 있다. In addition, conventional methods for producing nickel metal powder include a vapor phase method and a liquid phase method. The vapor phase method is a method of vaporizing nickel precursors to reduce and precipitate them, which is relatively easy to control impurities in powders, but has disadvantages such as high manufacturing cost, low productivity, and difficulty in entering language.

이에 비해 액상법은 초기 투자비와 공정 비용이 적다는 장점이 있으며 대량생산에도 유리하다. In contrast, the liquid phase method has the advantage of low initial investment and process cost, and is advantageous for mass production.

그리고, 액상법으로 제조되는 금속분말은 대부분 각 입자들이 서로 떨어져 있거나 뭉쳐있는 구조를 갖는데 이 금속분말을 사용하여 내부에 기공이 많은 소재를 만들기 위해서는 바인더와 같은 첨가제를 상당량 첨가해야 한다.And, most of the metal powder produced by the liquid phase method has a structure in which each particle is separated from each other or agglomerated. To use the metal powder to make a material having a lot of pores therein, a large amount of additives such as a binder must be added.

또한 금속분말 내부에 기공이 많을 경우에는 첨가하는 바인더양을 줄여 다공성 소재의 제조를 용이하게 할 수가 있고 열린 기공 구조를 쉽게 얻을 수 있어 다공성 소재의 제조 시 장점이 많게 된다.In addition, when there are a lot of pores in the metal powder, it is possible to reduce the amount of binder to be added to facilitate the manufacture of the porous material, and to easily obtain an open pore structure, thereby increasing the advantages of the porous material.

한편, 도전성 폴리머 제조를 위해 카본나노튜브 (carbon nanotube)나 금속분말을 충진제로 사용하는데 금속분말은 카본나노튜브에 비해 가격이 매우 저렴하다는 장점이 있다.Meanwhile, carbon nanotubes or metal powders are used as fillers for the production of conductive polymers. However, metal powders have the advantage of being very inexpensive compared to carbon nanotubes.

그러나 일반 구형 금속분말을 사용할 경우 폴리머 내부에서 분말입자 간의 연속적인 연결을 위해서 많은 양의 금속분말을 첨가하여야 하고 이로 인해 가격 상승하여 바람직하지 못하다.However, in the case of using a general spherical metal powder, a large amount of metal powder must be added for continuous connection between powder particles in the polymer, which increases the price and is not preferable.

또한, 분말입자의 첨가량이 많아지게 되면 폴리머와의 혼합이 난해한 문제점이 있다.In addition, when the amount of powder particles to be added increases, there is a problem that mixing with the polymer is difficult.

본 발명의 목적은 상기와 같은 종래의 문제점을 해결하기 위한 것으로, 습식법을 통해 제조하여 망목상의 입자구조를 가짐으로써 분말 내부 기공도가 증가하 며, 투자비와 공정 비용이 감소하도록 한 다공성 니켈 금속분말 및 이의 제조방법을 제공하는 것에 있다.An object of the present invention is to solve the conventional problems as described above, and the porous nickel metal powder made by the wet method has a mesh-like particle structure to increase the internal porosity of the powder, reducing the investment cost and process cost And a method for producing the same.

본 발명에 의한 다공성 니켈 금속분말은, 니켈 분말입자들 사이에 존재하는 인터스티셜포러시티(interstital porosity)를 제외한 니켈 분말입자 내부의 기공도가 2 내지 72%이며, 망목상 입자구조를 갖는 것을 특징으로 한다.The porous nickel metal powder according to the present invention has a porosity of 2 to 72% in the nickel powder particles except for interstital porosity present between the nickel powder particles, and has a mesh-like particle structure. It features.

본 발명에 의한 다공성 니켈 금속분말 제조방법은, 폴리올, 환원제, 니켈화합물 및 폴리머첨가제를 선택적으로 혼합하여 제1용액 및 제2용액을 형성하는 재료준비단계와: 상기 제2용액에 제1용액을 첨가하여 혼합용액을 형성하는 용액혼합단계와; 상기 혼합용액을 일정 온도로 가열하여 니켈 금속분말을 생성하는 니켈금속분말생성단계와; 상기 혼합용액에서 생성된 니켈 금속분말을 분리하는 니켈금속분말분리단계와; 분리된 니켈 금속분말을 세척 및 건조하는 니켈금속분말세척/건조단계로 이루어지는 것을 특징으로 한다.Method for preparing a porous nickel metal powder according to the present invention comprises the steps of preparing a material to form a first solution and a second solution by selectively mixing a polyol, a reducing agent, a nickel compound and a polymer additive: a first solution to the second solution A solution mixing step of adding to form a mixed solution; A nickel metal powder generation step of heating the mixed solution to a predetermined temperature to generate nickel metal powder; A nickel metal powder separation step of separating the nickel metal powder produced in the mixed solution; Characterized in that the nickel metal powder washing / drying step of washing and drying the separated nickel metal powder.

상기 재료준비단계는, 반응온도까지 가열된 폴리올과 환원제를 혼합하여 제1용액을 준비하는 제1용액준비과정과, 니켈화합물과 폴리머첨가제를 혼합하여 제2용액을 준비하는 제2용액준비과정을 포함하여 이루어진 것을 특징으로 한다.The material preparation step includes a first solution preparation process for preparing a first solution by mixing a polyol and a reducing agent heated to the reaction temperature, and a second solution preparation process for preparing a second solution by mixing a nickel compound and a polymer additive. Characterized in that the made up.

상기 제1용액준비과정에서, 상기 폴리올은 에틸렌글리콜 (ethylene glycol)을 포함하며, 디에틸렌글리콜 (diethylene glycol), 트리에틸렌글리콜 (triethylene glycol), 테트라에틸렌글리콜 (tetraethylene glycol), 디플필렌글리콜 (dipropylene glycol), 프로판디올 (propandiol), 부탄디올 (butanediol) 중 하 나 이상이 선택적으로 포함됨을 특징으로 한다.In the first solution preparation process, the polyol includes ethylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, and dipropylene glycol. One or more of glycol, propandiol and butanediol are selectively included.

상기 제1용액준비과정에서, 상기 환원제는 하이드라진, 하이드라진화합물, 하이드라진수화물 중 하나 이상을 포함하며, 소듐보로하이드라이드, 하이드로젠 설파이드, 하이드로젠 아이오다이드, 포스핀, 아신, 스티빈, 카본, 설퍼디옥사이드, 설파이트, 포스포러스산, 포스페이트, 하이드로포스포러스, 포타슘 시아나이드, 하이드라진, 포타슘 포메이트, 커프러스, 페러스, 코발터스 아민, 스태너스, 크로머스염, 메탈 소듐, 포타슘 중 하나 이상이 선택적으로 포함됨을 특징으로 한다.In the first solution preparation process, the reducing agent includes at least one of hydrazine, hydrazine compound, hydrazine hydrate, sodium borohydride, hydrogen sulfide, hydrogen iodide, phosphine, acine, styrene, carbon Sulfur dioxide, sulfite, phosphoric acid, phosphate, hydrophosphorus, potassium cyanide, hydrazine, potassium formate, cuff, ferrus, cobalt amine, stanus, chromus salt, metal sodium, potassium At least one is optionally included.

상기 제2용액준비과정에서, 상기 니켈화합물은 니켈클로라이드, 니켈클로라이드수화물, 니켈클로라이드화합물 중 하나 이상을 포함하며, 니켈니트레이트 (nickel nitrate), 니켈설페이트 (nickel sulfate), 니켈브로마이드 (nickel bromide), 니켈플루오라이드(nickel fluoride), 니켈아세테이트 (nickel acetate), 니켈아세틸아세토네이트 (nickel acetylacetonate), 니켈하이드록사이드 (nickel hydroxide), 니켈수산화물 중 하나 이상이 선택적으로 포함됨을 특징으로 한다.In the preparation of the second solution, the nickel compound includes at least one of nickel chloride, nickel chloride hydrate, and nickel chloride compound, and includes nickel nitrate, nickel sulfate, and nickel bromide. Nickel fluoride, nickel acetate, nickel acetylacetonate, nickel hydroxide, nickel hydroxide, and nickel hydroxide are optionally included.

상기 제2용액준비과정에서, 상기 폴리머첨가제는 폴리비닐피롤리돈 (polyvinylpyrrolidone, PVP)을 포함하며, 폴리비닐알콜 (polyvinylalchol, PVA), 공중합체 중 하나 이상이 선택적으로 포함됨을 특징으로 한다.In the second solution preparation process, the polymer additive includes polyvinylpyrrolidone (PVP), and is characterized in that one or more of polyvinyl alcohol (polyvinylalchol, PVA) and copolymers are optionally included.

상기 폴리올은 80 내지 250℃의 온도 범위 내에서 가열됨을 특징으로 한다.The polyol is characterized in that it is heated within a temperature range of 80 to 250 ℃.

상기 니켈금속분말생성단계에서 상기 혼합용액의 온도는 80 내지 250℃의 범위인 것을 특징으로 한다.In the nickel metal powder production step, the temperature of the mixed solution is characterized in that the range of 80 to 250 ℃.

상기 니켈금속분말세척/건조단계는, 분리된 니켈 금속분말을 알코올과 물 중 하나 이상을 포함하는 세척액에서 세척하는 과정임을 특징으로 한다.The nickel metal powder washing / drying step may be a process of washing the separated nickel metal powder in a washing solution including one or more of alcohol and water.

이와 같은 구성에 의하면, 초기 투자비와 공정 비용이 감소하며 대량생산이 가능한 이점이 있다.According to such a configuration, there is an advantage that the initial investment cost and the process cost can be reduced and mass production is possible.

이하에서는 첨부된 도 1을 참조하여 본 발명에 의한 다공성 니켈 금속분말의 제조방법을 설명한다.Hereinafter, with reference to the accompanying Figure 1 describes a method for producing a porous nickel metal powder according to the present invention.

도 1에는 본 발명에 의한 다공성 니켈 금속분말의 제조방법을 나타낸 제조공정도가 도시되어 있다.1 is a manufacturing process diagram showing a method for producing a porous nickel metal powder according to the present invention.

도면과 같이 본 발명에 의한 다공성 니켈 금속분말의 제조방법은, 폴리올, 환원제, 니켈화합물 및 폴리머첨가제를 선택적으로 혼합하여 제1용액 및 제2용액을 형성하는 재료준비단계(S100)와, 상기 제2용액에 제1용액을 첨가하여 혼합용액을 형성하는 용액혼합단계(S200)와; 상기 혼합용액을 일정 온도로 가열하여 니켈 금속분말을 생성하는 니켈금속분말생성단계(S300)와; 상기 혼합용액에서 생성된 니켈 금속분말을 분리하는 니켈금속분말분리단계(S400)와; 분리된 니켈 금속분말을 세척 및 건조하는 니켈금속분말세척/건조단계(S500)로 이루어진다.As shown in the drawing, the method for preparing a porous nickel metal powder according to the present invention includes preparing a material (S100) for forming a first solution and a second solution by selectively mixing a polyol, a reducing agent, a nickel compound, and a polymer additive, and A solution mixing step (S200) of forming a mixed solution by adding the first solution to the two solutions; A nickel metal powder producing step (S300) of heating the mixed solution to a predetermined temperature to generate nickel metal powder; Nickel metal powder separation step (S400) for separating the nickel metal powder produced in the mixed solution; Nickel metal powder washing / drying step of washing and drying the separated nickel metal powder (S500).

상기 재료준비단계(S100)을 보다 상세하게 살펴보면, 상기 재료준비단계(S100)는 반응온도까지 가열된 폴리올과 환원제를 혼합하여 제1용액을 준비하는 제1용액준비과정(S120)과, 니켈화합물과 폴리머첨가제를 혼합하여 제2용액을 준비하는 제2용액준비과정(S140)을 포함하여 이루어지며, 상기 제1용액준비과정(S120)과, 제2용액준비과정(S140)은 순서에 제한을 두지 않는다.Looking at the material preparation step (S100) in more detail, the material preparation step (S100) is a first solution preparation process (S120) for preparing a first solution by mixing a polyol and a reducing agent heated to the reaction temperature, and a nickel compound And a second solution preparation process (S140) of preparing a second solution by mixing a polymer additive with the first solution preparation process (S120) and the second solution preparation process (S140). Do not leave.

상기 제1용액준비과정(S120)은, 폴리올과 환원제를 섞어 제1용액을 만드는 과정으로, 상기 폴리올은 80 내지 250℃의 온도 범위까지 가열되며, 가열된 폴리올에 상기 환원제가 섞여 제1용액이 만들어지게 되며, 상기 제1용액에는 물이 선택적으로 혼합 가능하다.The first solution preparation process (S120) is a process of making a first solution by mixing a polyol and a reducing agent, the polyol is heated to a temperature range of 80 to 250 ℃, the reducing agent is mixed with the heated polyol the first solution is The first solution may be selectively mixed with water.

그리고, 상기 폴리올은 에틸렌글리콜 (ethylene glycol)을 포함하며, 디에틸렌글리콜 (diethylene glycol), 트리에틸렌글리콜 (triethylene glycol), 테트라에틸렌글리콜 (tetraethylene glycol), 디플필렌글리콜 (dipropylene glycol), 프로판디올 (propandiol), 부탄디올 (butanediol) 중 하나 이상이 선택적으로 포함된다.The polyol includes ethylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, dipropylene glycol, propanediol, and the like. propandiol) and butanediol are optionally included.

또한, 상기 환원제는 하이드라진, 하이드라진화합물, 하이드라진수화물 중 하나 이상을 포함하며, 소듐보로하이드라이드, 하이드로젠 설파이드, 하이드로젠 아이오다이드, 포스핀, 아신, 스티빈, 카본, 설퍼디옥사이드, 설파이트, 포스포러스산, 포스페이트, 하이드로포스포러스, 포타슘 시아나이드, 하이드라진, 포타슘 포메이트, 커프러스, 페러스, 코발터스 아민, 스태너스, 크로머스염, 메탈 소듐, 포타슘 중 하나 이상이 선택적으로 포함된다.In addition, the reducing agent includes at least one of hydrazine, hydrazine compound, hydrazine hydrate, sodium borohydride, hydrogen sulfide, hydrogen iodide, phosphine, asin, stibin, carbon, sulfoxide, sulfite Optionally include one or more of phosphoric acid, phosphate, hydrophosphorus, potassium cyanide, hydrazine, potassium formate, cuffus, ferrus, cobalt amine, stanus, chromus salt, metal sodium, potassium do.

상기와 같은 조성으로 제1용액이 만들어지면, 제2용액준비과정(S140)이 실시된다.When the first solution is made with the composition as described above, the second solution preparation process (S140) is performed.

상기 제2용액준비과정(S140)에서, 상기 니켈화합물은 니켈클로라이드나 니켈클로라이드헥사하이드레이트 (nickel chloride hexahydrate)를 포함하며, 니켈니트레이트 (nickel nitrate), 니켈설페이트 (nickel sulfate), 니켈브로마이드 (nickel bromide), 니켈플루오라이드(nickel fluoride), 니켈아세테이트 (nickel acetate), 니켈아세틸아세토네이트 (nickel acetylacetonate), 니켈하이드록사이드 (nickel hydroxide), 니켈수산화물 중 하나 이상이 선택적으로 포함된다.In the second solution preparation process (S140), the nickel compound includes nickel chloride or nickel chloride hexahydrate, nickel nitrate, nickel sulfate, and nickel bromide. bromide, nickel fluoride, nickel acetate, nickel acetylacetonate, nickel hydroxide, and nickel hydroxide are optionally included.

그리고, 상기 폴리머첨가제는 폴리비닐피롤리돈 (polyvinylpyrrolidone, PVP)을 포함하며, 폴리비닐알콜 (polyvinylalchol, PVA), 공중합체 중 하나 이상이 선택적으로 포함된다.In addition, the polymer additive includes polyvinylpyrrolidone (PVP), and optionally includes one or more of polyvinyl alcohol (polyvinylalchol, PVA) and a copolymer.

이때 상기 제2용액 제조를 위해 니켈화합물과 폴리머첨가제를 용매에 녹여 사용할 수도 있는데, 상기 용매로는 제1용액 제조시 사용된 폴리올 중 단독 또는 조합으로 사용이 가능하며, 보다 바람직하게는 에틸렌글리콜 단독 또는 에틸렌글리콜과 다른 폴리올과의 혼합물이 적용 가능하다. In this case, the nickel compound and the polymer additive may be dissolved in a solvent to prepare the second solution. The solvent may be used alone or in combination of polyols used in the preparation of the first solution, more preferably ethylene glycol alone. Or mixtures of ethylene glycol and other polyols are applicable.

상기 제2용액이 만들어져 재료준비단계(S100)가 완료되면, 상기 제1용액과 제2용액을 혼합하여 용액혼합단계(S200)를 실시한 후, 니켈금속분말생성단계(S300)가 이어지게 된다.When the second solution is made and the material preparation step (S100) is completed, the first solution and the second solution are mixed to perform a solution mixing step (S200), followed by the nickel metal powder production step (S300).

상기 니켈금속분말생성단계(S300)는 제1용액과 제2용액이 혼합된 혼합용액을 80 내지 250℃까지 가열한 후 일정 시간 동안 유지하여 니켈 금속분말을 생성하는 과정이다.The nickel metal powder production step (S300) is a process of generating nickel metal powder by heating the mixed solution in which the first solution and the second solution are mixed to 80 to 250 ° C. and maintaining the mixture for a predetermined time.

이후 상기 혼합용액으로부터 니켈 금속분말을 분리하여 니켈금속분말분리단계(S400)를 실시하게 되며, 분리된 니켈 금속분말은 니켈금속분말세척/건조단계(S500)에서 알코올과 물 중 하나 이상을 포함하는 세척액에서 세척된 후 50℃에서 건조하게 된다.Then, the nickel metal powder is separated from the mixed solution to perform a nickel metal powder separation step (S400), and the separated nickel metal powder includes one or more of alcohol and water in the nickel metal powder washing / drying step (S500). After washing in the washing liquid it is dried at 50 ℃.

본 발명에 의한 다공성 니켈 금속분말의 제조방법은 상기와 같은 단계에 따라 완료되며, 이하 본 발명의 실시예를 첨부된 도면을 토대로 설명하기로 한다.Method for producing a porous nickel metal powder according to the present invention is completed according to the steps as described above, will be described below with reference to the accompanying drawings an embodiment of the present invention.

[실시예 1]Example 1

용매인 에틸렌글리콜 300㎖를 195℃로 가열한 후 10분간 유지하였다. 80% 하이드라진모노하이드레이트 (hydrazine monohydrate) 30㎖를 증류수 30㎖에 첨가한 혼합용액을 상기 에틸렌글리콜 용액에 천천히 첨가하여 제1용액을 제조한 후 5분간 유지하였다.(제1용액준비과정:S120)300 ml of a solvent, ethylene glycol, was heated to 195 ° C. and held for 10 minutes. A mixed solution, in which 30 ml of 80% hydrazine monohydrate was added to 30 ml of distilled water, was slowly added to the ethylene glycol solution to prepare a first solution and maintained for 5 minutes. (First solution preparation process: S120)

니켈클로라이드헥사하이드레이트 (nickel chloride hexahydrate) 3.57g을 에틸렌글리콜 150㎖에 녹인 용액과 평균분자량이 55,000인 폴리비닐피롤리돈 1.67g을 에틸렌글리콜 300㎖에 녹인 용액을 혼합하여 제2용액을 제조한 후(제2용액준비과정:S140) 이를 제1용액에 투입하여 혼합하였다(용액혼합단계:S200).3.57 g of nickel chloride hexahydrate was dissolved in 150 ml of ethylene glycol, and a solution of 1.67 g of polyvinylpyrrolidone having an average molecular weight of 55,000 was dissolved in 300 ml of ethylene glycol, thereby preparing a second solution. (Second solution preparation process: S140) This was added to the first solution and mixed (solution mixing step: S200).

상기 혼합용액을 195℃에서 1시간 동안 반응하여 니켈 금속분말을 생성시키고(니켈금속분말생성단계:S300), 상기 니켈 금속분말을 용액으로부터 분리한 후(니켈금속분말분리단계:S400), 이 분말을 수거하여 에탄올로 세척, 여과한 후 50℃에서 건조하였다(니켈금속분말세척/건조단계:S500).  The mixed solution was reacted for 1 hour at 195 ° C. to produce nickel metal powder (nickel metal powder production step: S300), and the nickel metal powder was separated from the solution (nickel metal powder separation step: S400), and then the powder It was collected, washed with ethanol, filtered and dried at 50 ° C. (nickel metal powder washing / drying step: S500).

도 2는 본 발명의 제1실시예에 따라 제조된 다공성 니켈 금속분말의 주사전자현미경 사진으로서, 니켈 금속분말 입자들이 망목상의 구조를 나타낸 것을 알 수 있으며, 이러한 망목상의 구조로 니켈 금속분말 내에는 많은 기공이 존재 가능하다. Figure 2 is a scanning electron micrograph of the porous nickel metal powder prepared according to the first embodiment of the present invention, it can be seen that the nickel metal powder particles exhibit a network structure, such a network structure in the nickel metal powder Many pores are possible.

[실시예 2]Example 2

[실시예 2]에서는 [실시예 1]과 동일한 제조방법을 사용하였으며 다만, 평균분자량이 55,000인 폴리비닐피롤리돈의 양을 각각 각각 0g, 0.67g, 3.33g, 16.65g로 달리하여 첨가한 니켈 금속분말을 제조하고, 수은기공계를 사용하여 기공도를 측정하였다. In Example 2, the same production method as in Example 1 was used, except that polyvinylpyrrolidone having an average molecular weight of 55,000 was added in different amounts of 0g, 0.67g, 3.33g, and 16.65g, respectively. Nickel metal powder was prepared, and porosity was measured using a mercury porosimetry.

도 3은 본 발명의 제1실시예 및 제2실시예에 따라 제조된 다공성 니켈 금속분말의 기공도(porosity) 변화를 보인 그래프로서, 기공도는 니켈 금속분말 시료 전체에 대한 총기공도에서 분말입자 내부에 존재하지 않고 2차입자와 2차입자들 사이에 존재하는 인터스티셜포러시티(interstital porosity)를 뺀 실제 기공도를 나타낸 것이다.Figure 3 is a graph showing the porosity (porosity) change of the porous nickel metal powder prepared according to the first and second embodiments of the present invention, the porosity is powder particles in the total porosity for the entire nickel metal powder sample It shows the actual porosity minus the interstitial porosity that does not exist inside and exists between the secondary particles and the secondary particles.

도 3과 같이 기공도는 폴리비닐피롤리돈의 첨가량이 증가함에 따라 증가하다가 폴리비닐피롤리돈의 첨가량이 3.33g 이상에서는 더 이상 기공도가 증가하지 않고 일정한 값을 나타내었다. As shown in FIG. 3, the porosity increases with an increase in the amount of polyvinylpyrrolidone added, but when the amount of polyvinylpyrrolidone added is 3.33 g or more, the porosity does not increase any more and has a constant value.

[실시예 3]Example 3

[실시예 3]은 [실시예 1]과 동일한 제조방법을 사용하였으며, 다만 니켈클로라이드헥사하이드레이트의 첨가량은 [실시예 1] 보다 10배 많은 35.7g을 사용하였다. 그리고, 폴리비닐피롤리돈을 9.99g 사용하였다. [Example 3] used the same production method as in [Example 1], except that 35.7 g of nickel chloride hexahydrate was added 10 times more than [Example 1]. And 9.99g of polyvinylpyrrolidone was used.

즉, 용매인 에틸렌글리콜 300㎖를 195℃로 가열한 후 그 온도에서 10분간 유 지하였다. 80% 하이드라진모노하이드레이트 (hydrazine monohydrate) 30㎖를 증류수 30㎖에 첨가한 혼합용액을 상기 에틸렌글리콜 용액에 천천히 첨가하여 제1용액을 제조한 후 5분간 유지하였다.That is, 300 ml of a solvent, ethylene glycol, was heated to 195 ° C. and maintained at that temperature for 10 minutes. A mixed solution, in which 30 ml of 80% hydrazine monohydrate was added to 30 ml of distilled water, was slowly added to the ethylene glycol solution to prepare a first solution, and then maintained for 5 minutes.

니켈클로라이드헥사하이드레이트(nickel chloride hexahydrate)는 [실시예 1] 보다 10배 많은 35.7g을 에틸렌글리콜 150㎖에 녹인 용액과 평균분자량이 55,000인 폴리비닐피롤리돈 9.99g을 에틸렌글리콜 300㎖에 녹인 용액을 혼합하여 제2용액을 제조한 후 이를 제1용액에 투입하여 혼합하였다.Nickel chloride hexahydrate is a solution in which 35.7 g of 10 times more than [Example 1] is dissolved in 150 ml of ethylene glycol and 9.99 g of polyvinylpyrrolidone having an average molecular weight of 55,000 in 300 ml of ethylene glycol. To prepare a second solution by mixing the mixture was added to the first solution and mixed.

이 혼합용액을 195℃에서 1시간 동안 반응시켜 니켈 금속분말을 생성시키고 이 분말을 수거하여 에탄올로 세척, 여과한 후 50℃에서 건조하였다.The mixed solution was reacted at 195 ° C. for 1 hour to produce nickel metal powder. The powder was collected, washed with ethanol, filtered, and dried at 50 ° C.

도 4는 본 발명의 제3실시예에 따라 제조된 다공성 니켈 금속분말의 주사전자현미경 사진으로서, 니켈 금속분말의 입자들이 망목상의 구조를 나타내는 것을 알 수있으며, 이러한 망목상의 입자들은 니켈 분말 내에 많은 기공을 형성한 것을 확인 할 수 있다.  Figure 4 is a scanning electron micrograph of the porous nickel metal powder prepared according to the third embodiment of the present invention, it can be seen that the particles of the nickel metal powder exhibits a network structure, these mesh particles are found in the nickel powder You can see that the pores formed.

[실시예 4]Example 4

[실시예 4]에서는 [실시예 1]과 동일한 제조방법을 사용하되 폴리비닐피롤리돈은 3.33g 첨가하였으며, 반응온도를 100℃로 하여 니켈 금속분말을 제조하였다. In [Example 4], using the same production method as in [Example 1], 3.33g of polyvinylpyrrolidone was added, and a nickel metal powder was prepared at a reaction temperature of 100 ° C.

용매인 에틸렌글리콜 300㎖를 100℃로 가열한 후 그 온도에서 10분간 유지하였다. 80% 하이드라진모노하이드레이트 (hydrazine monohydrate) 30㎖를 증류수 30㎖에 첨가한 혼합 용액을 상기의 에틸렌글리콜 용액에 천천히 첨가하여 제 1 용액 을 제조한 후 5분간 유지하였다.300 ml of a solvent, ethylene glycol, was heated to 100 ° C., and then maintained at that temperature for 10 minutes. A mixed solution, in which 30 ml of 80% hydrazine monohydrate was added to 30 ml of distilled water, was slowly added to the ethylene glycol solution to prepare a first solution, and then maintained for 5 minutes.

니켈클로라이드헥사하이드레이트 (nickel chloride hexahydrate) 3.57g을 에틸렌글리콜 150㎖에 녹인 용액과 평균분자량이 55,000인 폴리비닐피롤리돈을 3.33g을 에틸렌글리콜 300㎖에 녹인 용액을 혼합하여 제2용액을 제조한 후 이를 제 1 용액에 투입하여 혼합하였다.A second solution was prepared by mixing a solution of 3.57 g of nickel chloride hexahydrate in 150 ml of ethylene glycol and a solution of 3.33 g of polyvinylpyrrolidone having an average molecular weight of 55,000 in 300 ml of ethylene glycol. It was then added to the first solution and mixed.

이 혼합용액을 100℃에서 1시간 동안 반응하여 니켈분말을 생성시키고 이 분말을 수거하여 에탄올로 세척, 여과한 후 50℃에서 건조하였다. The mixed solution was reacted at 100 ° C. for 1 hour to form nickel powder. The powder was collected, washed with ethanol, filtered, and dried at 50 ° C.

도 5는 본 발명의 제4실시예에 따라 제조된 다공성 니켈 금속분말의 주사전자현미경 사진으로서 니켈 금속분말의 입자들이 망목상의 구조를 나타내는 것을 알 수 있다.Figure 5 is a scanning electron micrograph of the porous nickel metal powder prepared according to the fourth embodiment of the present invention can be seen that the particles of the nickel metal powder exhibits a network structure.

그리고, [실시예 1]에서 반응온도 195℃에서 제조된 니켈 금속분말의 입자 표면은 매끄러운 반면 [실시예 4]에서 반응온도 100℃로 제조된 니켈 금속분말의 입자 표면은 거친편이었다.In addition, the particle surface of the nickel metal powder prepared at the reaction temperature of 195 ° C. in [Example 1] was smooth, whereas the particle surface of the nickel metal powder prepared at the reaction temperature of 100 ° C. in [Example 4] was coarse.

[실시예 5]Example 5

[실시예 5]는 [실시예 1]과 동일한 제조방법을 사용하였으되 평균분자량이 실시예1보다 매우 큰 1,300,000인 폴리비닐피롤리돈 3.33g을 사용하여 니켈분말을 제조한 예이다. [Example 5] is an example in which nickel powder was prepared using the same production method as in [Example 1], but using 3.33 g of polyvinylpyrrolidone having an average molecular weight of 1,300,000, which is much larger than that of Example 1.

용매인 에틸렌글리콜 300㎖를 195℃로 가열한 후 그 온도에서 10분간 유지하였다. 80% 하이드라진모노하이드레이트 (hydrazine monohydrate) 30㎖를 증류수 30 ㎖에 첨가한 혼합용액을 상기의 에틸렌글리콜 용액에 천천히 첨가하여 제1용액을 제조한 후 5분간 유지하였다.300 ml of a solvent, ethylene glycol, was heated to 195 ° C. and maintained at that temperature for 10 minutes. A mixed solution, in which 30 ml of 80% hydrazine monohydrate was added to 30 ml of distilled water, was slowly added to the ethylene glycol solution to prepare a first solution, and then maintained for 5 minutes.

니켈클로라이드헥사하이드레이트 (nickel chloride hexahydrate) 3.57g을 에틸렌글리콜 150㎖에 녹인 용액과 평균분자량이 1,300,000인 폴리비닐피롤리돈 3.33g을 에틸렌글리콜 300㎖에 녹인 용액을 혼합하여 제2용액을 제조한 후 이를 제1용액에 투입하여 혼합하였다.A second solution was prepared by mixing a solution of 3.57 g of nickel chloride hexahydrate in 150 ml of ethylene glycol and a solution of 3.33 g of polyvinylpyrrolidone having an average molecular weight of 1,300,000 in 300 ml of ethylene glycol. This was added to the first solution and mixed.

이 혼합용액을 195℃에서 1시간 동안 반응하여 니켈 금속분말을 생성시키고 이 니켈 금속분말을 수거하여 에탄올로 세척, 여과한 후 50℃에서 건조하였다. The mixed solution was reacted at 195 ° C. for 1 hour to produce nickel metal powder. The nickel metal powder was collected, washed with ethanol, filtered, and dried at 50 ° C.

도 6은 본 발명의 제5실시예에 따라 제조된 다공성 니켈 금속분말의 주사전자현미경 사진으로서 니켈 금속분의 입자들이 망목상의 구조를 나타내는 것을 알 수 있으며, 이러한 망목상의 구조로 니켈 금속분말 내에 많은 기공이 존재하게 됨을 확인할 수 있다.6 is a scanning electron micrograph of the porous nickel metal powder prepared according to the fifth embodiment of the present invention, and it can be seen that the particles of the nickel metal powder exhibit a network structure, and the pores in the nickel metal powder have a network structure. You can see that this exists.

그리고, [실시예 1]에서 반응온도 195oC로 제조된 니켈 금속분말의 입자 표면은 매끄러운 반면 [실시예 5]에 의해 반응온도 100oC로 제조된 니켈 금속분말의 입자 표면은 거친 편이었다.In addition, the particle surface of the nickel metal powder prepared at the reaction temperature of 195 o C in [Example 1] was smooth, whereas the particle surface of the nickel metal powder prepared at the reaction temperature of 100 o C according to [Example 5] was rough. .

[비교예 1]Comparative Example 1

[비교예 1]에서 [실시예 1]과 동일한 제조방법을 사용하되 폴리비닐피롤리돈을 첨가하지 않고 니켈 금속분말을 제조한 예이다. In Comparative Example 1, a nickel metal powder was prepared using the same production method as in Example 1 without adding polyvinylpyrrolidone.

즉, 용매인 에틸렌글리콜 300㎖를 195℃로 가열한 후 그 온도에서 10분간 유지하였다. 80% 하이드라진모노하이드레이트 (hydrazine monohydrate) 30㎖를 증류수 30㎖에 첨가한 혼합 용액을 상기의 에틸렌글리콜 용액에 천천히 첨가하여 제1용액을 제조한 후 5분간 유지하였다.That is, 300 ml of a solvent, ethylene glycol, was heated to 195 ° C. and maintained at that temperature for 10 minutes. A mixed solution, in which 30 ml of 80% hydrazine monohydrate was added to 30 ml of distilled water, was slowly added to the ethylene glycol solution to prepare a first solution, and then maintained for 5 minutes.

이후 니켈클로라이드헥사하이드레이트 (nickel chloride hexahydrate) 3.57g을 에틸렌글리콜 150㎖에 녹인 용액을 제조한 후 이를 제1용액에 투입하여 혼합하였다. Thereafter, a solution of 3.57 g of nickel chloride hexahydrate dissolved in 150 ml of ethylene glycol was prepared, and this was added to the first solution and mixed.

그리고, 상기의 [실시예] 에서 첨가한 폴리비닐피롤리돈을 첨가하지 않았다. 상기 혼합용액을 195℃에서 1시간 동안 반응시켜 니켈 금속분말을 생성시키고 이 분말을 수거하여 에탄올로 세척, 여과한 후 50℃에서 건조하였다.And the polyvinylpyrrolidone added in said Example was not added. The mixed solution was reacted at 195 ° C. for 1 hour to produce nickel metal powder. The powder was collected, washed with ethanol, filtered, and dried at 50 ° C.

그 결과, 도 7과 같이 니켈 금속분말의 입자는 망목상의 구조를 나타내지 않고 뭉쳐져 있는 구조를 나타낸 것을 확인할 수 있다.As a result, as shown in FIG. 7, the particles of the nickel metal powder did not show the network structure but showed the aggregated structure.

도 7은 본 발명에 의한 다공성 니켈 금속분말에 대한 제1비교예의 주사전자현미경 사진이다.7 is a scanning electron micrograph of the first comparative example for the porous nickel metal powder according to the present invention.

[비교예 2]Comparative Example 2

[비교예 2]는 [실시예 1]과 동일한 제조방법을 사용하였으며, 다만 폴리비닐피롤리돈을 첨가하지 않고 평균분자량이 1,500인 폴리비닐알콜 1.32g을 첨가하여 니켈 금속분말을 제조한 예이다. [Comparative Example 2] used the same production method as in [Example 1], except that 1.32 g of polyvinyl alcohol having an average molecular weight of 1,500 was added without adding polyvinylpyrrolidone to prepare nickel metal powder. .

용매인 에틸렌글리콜 300㎖를 195℃로 가열한 후 그 온도에서 10분간 유지하 였다. 80% 하이드라진모노하이드레이트 (hydrazine monohydrate) 30㎖를 증류수 30㎖에 첨가한 혼합 용액을 상기의 에틸렌글리콜 용액에 천천히 첨가하여 제 1 용액을 제조한 후 5분간 유지하였다.300 ml of a solvent, ethylene glycol, was heated to 195 ° C. and maintained at that temperature for 10 minutes. A mixed solution, in which 30 ml of 80% hydrazine monohydrate was added to 30 ml of distilled water, was slowly added to the ethylene glycol solution to prepare a first solution, and then maintained for 5 minutes.

니켈클로라이드헥사하이드레이트 (nickel chloride hexahydrate) 3.57g을 에틸렌글리콜 150㎖에 녹인 용액과 평균분자량이 1,500인 폴리비닐알콜 1.32g을 에틸렌글리콜 300㎖에 녹인 용액을 혼합하여 제2용액을 제조한 후 이를 제1용액에 투입하여 혼합하였다.3.57 g of nickel chloride hexahydrate was dissolved in 150 ml of ethylene glycol, and a solution of 1.32 g of polyvinyl alcohol having an average molecular weight of 1,500 was dissolved in 300 ml of ethylene glycol to prepare a second solution. 1 solution was added and mixed.

이 혼합용액을 195℃에서 1시간 동안 반응하여 니켈분말을 생성시키고 이 분말을 수거하여 에탄올로 세척, 여과한 후 50℃에서 건조하였다. The mixed solution was reacted at 195 ° C. for 1 hour to produce nickel powder. The powder was collected, washed with ethanol, filtered, and dried at 50 ° C.

도 8과 같이 폴리비닐피롤리돈을 첨가하지 않고 평균분자량이 1,500인 폴리비닐알콜 1.32g을 첨가하여 니켈 금속분말을 제조한 경우, 니켈 금속분말의 입자들이 망목상의 구조를 나타내지 않는 것을 확인할 수 있다.When the nickel metal powder was prepared by adding 1.32 g of polyvinyl alcohol having an average molecular weight of 1,500 without adding polyvinylpyrrolidone as shown in FIG. 8, it can be seen that the particles of the nickel metal powder do not exhibit a network structure. .

도 8은 본 발명에 의한 다공성 니켈 금속분말에 대한 제2비교예의 주사전자현미경 사진이다.8 is a scanning electron micrograph of a second comparative example for the porous nickel metal powder according to the present invention.

이러한 본 발명의 범위는 상기에서 예시한 실시예에 한정하지 않고, 상기와 같은 기술범위 안에서 당업계의 통상의 기술자에게 있어서는 본 발명을 기초로 하는 다른 많은 변형이 가능할 것이다.The scope of the present invention is not limited to the above-exemplified embodiments, and many other modifications based on the present invention may be made by those skilled in the art within the above technical scope.

본 발명에 의한 다공성 니켈 금속분말은 입도가 미세하고 균일하며 망목상의 구조를 갖는 이점이 있다. Porous nickel metal powder according to the present invention has the advantage that the particle size is fine, uniform and has a network structure.

또한, 본 발명에 의한 니켈 금속분말 제조방법에 따르면, 내부에 많은 기공을 포함하고 있으므로 연료전지용 전극, 이차전지용 전극, 전도성폴리머 제조를 위한 금속충진제, 촉매소재, 필터 등의 다양한 용도에 적용 가능한 이점이 있다.In addition, according to the method for producing nickel metal powder according to the present invention, since it contains many pores therein, it is possible to apply to various applications such as fuel cell electrodes, secondary battery electrodes, metal fillers for the production of conductive polymers, catalyst materials, filters, and the like. There is this.

뿐만 아니라, 초기 투자비와 공정 비용이 감소하며 대량생산이 가능한 이점이 있다.In addition, there is an advantage that the initial investment and processing costs are reduced and mass production is possible.

Claims (10)

니켈 분말입자들 사이에 존재하는 인터스티셜포러시티(interstital porosity)를 제외한 니켈 분말입자 내부의 기공도가 2 내지 72%이며, 망목상 입자구조를 갖는 것을 특징으로 하는 다공성 니켈 금속분말.A porous nickel metal powder having a porosity of 2 to 72% except for interstital porosity present between the nickel powder particles, and having a mesh-like particle structure. 폴리올, 환원제, 니켈화합물 및 폴리머첨가제를 선택적으로 혼합하여 제1용액 및 제2용액을 형성하는 재료준비단계와,A material preparation step of selectively mixing a polyol, a reducing agent, a nickel compound and a polymer additive to form a first solution and a second solution, 상기 제2용액에 제1용액을 첨가하여 혼합용액을 형성하는 용액혼합단계와;A solution mixing step of forming a mixed solution by adding a first solution to the second solution; 상기 혼합용액을 일정 온도로 가열하여 니켈 금속분말을 생성하는 니켈금속분말생성단계와;A nickel metal powder generation step of heating the mixed solution to a predetermined temperature to generate nickel metal powder; 상기 혼합용액에서 생성된 니켈 금속분말을 분리하는 니켈금속분말분리단계와;A nickel metal powder separation step of separating the nickel metal powder produced in the mixed solution; 분리된 니켈 금속분말을 세척 및 건조하는 니켈금속분말세척/건조단계로 이루어지는 것을 특징으로 하는 다공성 니켈금속분말의 제조방법.Method for producing a porous nickel metal powder, characterized in that the nickel metal powder washing / drying step of washing and drying the separated nickel metal powder. 제 2 항에 있어서, 상기 재료준비단계는,The method of claim 2, wherein the material preparation step, 반응온도까지 가열된 폴리올과 환원제를 혼합하여 제1용액을 준비하는 제1용액준비과정과,A first solution preparation process of preparing a first solution by mixing a polyol heated to a reaction temperature and a reducing agent; 니켈화합물과 폴리머첨가제를 혼합하여 제2용액을 준비하는 제2용액준비과정 을 포함하여 이루어진 것을 특징으로 하는 다공성 니켈금속분말의 제조방법.A method of producing a porous nickel metal powder, comprising the step of preparing a second solution by mixing a nickel compound and a polymer additive. 제 2 항에 있어서, 상기 제1용액준비과정에서,The method of claim 2, wherein in the first solution preparation process, 상기 폴리올은 에틸렌글리콜 (ethylene glycol)을 포함하며,The polyol includes ethylene glycol, 디에틸렌글리콜 (diethylene glycol), 트리에틸렌글리콜 (triethylene glycol), 테트라에틸렌글리콜 (tetraethylene glycol), 디플필렌글리콜 (dipropylene glycol), 프로판디올 (propandiol), 부탄디올 (butanediol) 중 하나 이상이 선택적으로 포함됨을 특징으로 하는 다공성 니켈 금속분말의 제조방법.May optionally include one or more of diethylene glycol, triethylene glycol, tetraethylene glycol, dipropylene glycol, propandiol and butanediol. Method for producing a porous nickel metal powder, characterized in that. 제 2 항에 있어서, 상기 제1용액준비과정에서,The method of claim 2, wherein in the first solution preparation process, 상기 환원제는 하이드라진, 하이드라진화합물, 하이드라진수화물 중 하나 이상을 포함하며, The reducing agent includes at least one of hydrazine, hydrazine compound, hydrazine hydrate, 소듐보로하이드라이드, 하이드로젠 설파이드, 하이드로젠 아이오다이드, 포스핀, 아신, 스티빈, 카본, 설퍼디옥사이드, 설파이트, 포스포러스산, 포스페이트, 하이드로포스포러스, 포타슘 시아나이드, 하이드라진, 포타슘 포메이트, 커프러스, 페러스, 코발터스 아민, 스태너스, 크로머스염, 메탈 소듐, 포타슘 중 하나 이상이 선택적으로 포함됨을 특징으로 하는 다공성 니켈 금속분말의 제조방법.Sodium borohydride, hydrogen sulfide, hydrogen iodide, phosphine, amine, styrene, carbon, sulfur dioxide, sulfite, phosphoric acid, phosphate, hydrophosphorus, potassium cyanide, hydrazine, potassium phosphorus A method for producing a porous nickel metal powder, characterized in that one or more of mate, cuff, ferrus, cobalt amine, stanus, chromus salt, metal sodium, potassium is optionally included. 제 2 항에 있어서, 상기 제2용액준비과정에서,The method of claim 2, wherein in the preparation of the second solution, 상기 니켈화합물은 니켈클로라이드, 니켈클로라이드수화물, 니켈클로라이드 화합물 중 하나 이상을 포함하며,The nickel compound includes one or more of nickel chloride, nickel chloride hydrate, nickel chloride compound, 니켈니트레이트 (nickel nitrate), 니켈설페이트 (nickel sulfate), 니켈브로마이드 (nickel bromide), 니켈플루오라이드(nickel fluoride), 니켈아세테이트 (nickel acetate), 니켈아세틸아세토네이트 (nickel acetylacetonate), 니켈하이드록사이드 (nickel hydroxide), 니켈수산화물 중 하나 이상이 선택적으로 포함됨을 특징으로 하는 다공성 니켈 금속분말의 제조방법.Nickel nitrate, nickel sulfate, nickel bromide, nickel fluoride, nickel acetate, nickel acetylacetonate, nickel hydroxide (nickel hydroxide), a method for producing a porous nickel metal powder, characterized in that it optionally comprises at least one of nickel hydroxide. 제 2 항에 있어서, 상기 제2용액준비과정에서,The method of claim 2, wherein in the preparation of the second solution, 상기 폴리머첨가제는 폴리비닐피롤리돈 (polyvinylpyrrolidone, PVP)을 포함하며,The polymer additive includes polyvinylpyrrolidone (PVP), 폴리비닐알콜 (polyvinylalchol, PVA), 공중합체 중 하나 이상이 선택적으로 포함됨을 특징으로 하는 다공성 니켈 금속분말의 제조방법.Polyvinyl alcohol (polyvinylalchol, PVA), a method for producing a porous nickel metal powder, characterized in that it is optionally included. 제 2 항 내지 제 7 항 중 어느 한 항에 있어서, 상기 폴리올은 80 내지 250℃의 온도 범위 내에서 가열됨을 특징으로 하는 다공성 니켈 금속분말의 제조방법. 8. The method of claim 2, wherein the polyol is heated within a temperature range of 80 to 250 ° C. 9. 제 2 항 내지 제 7 항 중 어느 한 항에 있어서, 상기 니켈금속분말생성단계에서 상기 혼합용액의 온도는 80 내지 250℃의 범위인 것을 특징으로 하는 다공성 니켈 금속분말의 제조방법.The method of claim 2, wherein the temperature of the mixed solution in the nickel metal powder producing step is in a range of 80 to 250 ° C. 9. 제 2 항 내지 제 7 항 중 어느 한 항에 있어서, 상기 니켈금속분말세척/건조단계는, 분리된 니켈 금속분말을 알코올과 물 중 하나 이상을 포함하는 세척액에서 세척하는 과정임을 특징으로 하는 다공성 니켈 금속분말 및 이의 제조방법.8. The porous nickel according to any one of claims 2 to 7, wherein the washing / drying of the nickel metal powder is a process of washing the separated nickel metal powder in a washing solution containing at least one of alcohol and water. Metal powder and its manufacturing method.
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