[go: up one dir, main page]

KR101156509B1 - The carbon foam having a nickel coating layer and method for manufacturing same - Google Patents

The carbon foam having a nickel coating layer and method for manufacturing same Download PDF

Info

Publication number
KR101156509B1
KR101156509B1 KR1020100042958A KR20100042958A KR101156509B1 KR 101156509 B1 KR101156509 B1 KR 101156509B1 KR 1020100042958 A KR1020100042958 A KR 1020100042958A KR 20100042958 A KR20100042958 A KR 20100042958A KR 101156509 B1 KR101156509 B1 KR 101156509B1
Authority
KR
South Korea
Prior art keywords
carbon foam
plating layer
nickel plating
pores
hydrophilization
Prior art date
Application number
KR1020100042958A
Other languages
Korean (ko)
Other versions
KR20110123460A (en
Inventor
임영목
김두현
이재호
Original Assignee
한국기계연구원
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 한국기계연구원 filed Critical 한국기계연구원
Priority to KR1020100042958A priority Critical patent/KR101156509B1/en
Publication of KR20110123460A publication Critical patent/KR20110123460A/en
Application granted granted Critical
Publication of KR101156509B1 publication Critical patent/KR101156509B1/en

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • C04B41/88—Metals
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D1/00—Electroforming
    • C25D1/08—Perforated or foraminous objects, e.g. sieves
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/54—Electroplating of non-metallic surfaces

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Structural Engineering (AREA)
  • Chemically Coating (AREA)

Abstract

본 발명에 의한 니켈도금층이 구비된 탄소폼은, 기공이 형성되고 친수성을 가지는 탄소폼과, 상기 기공의 표면에 코팅된 니켈도금층을 포함하여 구성된다. 본 발명에 의한 니켈도금층이 구비된 탄소폼의 제조방법은, 다수 기공이 형성된 탄소폼을 암모니아에 침적하여 친수화 처리하는 탄소폼친수화단계와, 친수화 처리된 탄소폼을 무전해도금법으로 니켈도금층을 형성하는 니켈도금층형성단계로 이루어지는 것을 특징으로 한다.Carbon foam having a nickel plated layer according to the present invention comprises a carbon foam having pores and hydrophilicity, and a nickel plated layer coated on the surface of the pores. The method for producing a carbon foam with a nickel plating layer according to the present invention includes a carbon foam hydrophilization step of hydrophilizing a carbon foam having a plurality of pores formed therein with ammonia, and a nickel plating layer by electroless plating the hydrophilized carbon foam. Characterized in that the nickel plating layer forming step of forming a.

Description

니켈도금층이 구비된 탄소폼 및 이의 제조방법{The carbon foam having a nickel coating layer and method for manufacturing same}The carbon foam having a nickel coating layer and method for manufacturing same

본 발명은 다공성 탄소폼을 암모니아 용액에서 친수화 처리하고, 친수 처리된 다공성 탄소폼에 나켈도금층이 형성되도록 한 니켈도금층이 구비된 탄소폼 및 이의 제조방법에 관한 것이다.The present invention relates to a carbon foam having a nickel plating layer and a method of manufacturing the same, which are made to hydrophilize the porous carbon foam in an ammonia solution, and a nickel plating layer is formed on the hydrophilic porous carbon foam.

다공성 구조를 가진 금속폼은 디젤자동차의 매연저감장치(DBF), 소각로 및 발전소용 필터, 배기가스 정화용 촉매담체, 전극소재 등에 사용되는 소재로 환경,에너지 산업 등 녹색산업에 필수적인 소재이다.Metal foam with porous structure is used for diesel particulate filter (DBF), incinerator and power plant filter, exhaust gas purification catalyst carrier, electrode material, etc., which is essential for green industry such as environment, energy industry.

기공이 서로 연통된 개기공 구조를 가진 금속폼을 제조하는 기존의 대표적인 방법은 폴리우레탄 폼의 표면에 물리적 증기 증착법 (PVD, Physical Vapour Deposition)으로 Ni 층을 형성시킨 후 전해도금 등을 통해 Ni 층을 성장시키는 방법이다.The conventional representative method for manufacturing a metal foam having an open pore structure in which the pores are in communication with each other is to form a Ni layer on the surface of the polyurethane foam by physical vapor deposition (PVD, Physical Vapor Deposition) and then Ni layer through electroplating. How to grow.

그러나 상기 방법은 물리적 증기 증착법 등 복잡한 공정을 요구하고, 기공이 미세할 경우 표면과 내부의 증착율이 달라 두께가 두꺼운 다공성 폼의 제조에 어려움이 있다.However, the method requires a complicated process such as a physical vapor deposition method, and when the pores are fine, it is difficult to prepare a porous foam having a thick thickness due to different deposition rates on the surface and the inside.

또한 형틀로 사용하는 폴리우레탄 폼의 내열온도가 낮아 고온의 사용환경에서는 폴리우레탄이 기화되므로 일반적으로 생산공정동안에 기화시킴으로써 최종제품에는 폴리우레탄이 존재하던 자리에 미세한 기공형태가 남게 되며, 구조적 강도저하를 유발하게 된다. In addition, the polyurethane foam used as a mold has a low heat resistance temperature, so that polyurethane is vaporized in a high-temperature operating environment, so that it is generally vaporized during the production process, so that a fine pore form remains in the place where the polyurethane existed in the final product, and structural strength decreases. Will cause.

따라서 고온 진공분위기에서 화학적 및 물리적으로 안정한 탄소 다공체를 지지체로 이용하여 그 표면에 니켈을 무전해 도금방법으로 형성시키면 기존의 금속 폼이 사용되는 거의 모든 분야에 적용될 수 있으며, 내산화성, 촉매특성 등 필요한 용도에 따라 적절한 합금을 Ni 도금층 위에 추가로 성장시켜 사용할 수 있다. Therefore, by using chemically and physically stable carbon porous body as a support in the high temperature vacuum atmosphere and forming nickel on its surface by electroless plating method, it can be applied to almost all fields where existing metal foam is used. Depending on the required application, an appropriate alloy can be further grown and used on the Ni plating layer.

이외에도 탄소를 고온산화분위기에서 기화시킴으로써 지지체 부분을 추가적인 기공으로 바꿀 수도 있다.In addition, by evaporating carbon in a high temperature oxidation atmosphere, the support portion may be converted into additional pores.

그러나 탄소계 물질의 경우, 일반적으로 소수성을 나타내므로 다공체 내의 기공에 무전해 도금 용액이 골고루 침투하기 위해서는 친수화 처리가 필요하다.However, in the case of the carbon-based material, since it is generally hydrophobic, hydrophilization treatment is required to evenly infiltrate the electroless plating solution into the pores in the porous body.

종래에는 탄소계 소재의 친수화 처리를 위해 반응성 가스를 이용한 플라즈마 전처리를 실시함으로써 표면이 개질될 수 있도록 하였다.Conventionally, the surface may be modified by performing plasma pretreatment using a reactive gas for hydrophilization of carbon-based materials.

그러나, 이러한 플라즈마 친수화 처리 공정은 비용이 많이 들며 후속공정으로 습식분위기에서 무전해도금을 진행해야한다는 점을 고려하면, 진공 건식 공정 후 습식 공정으로 진행되어야 하므로 공정이 복잡하고 시간에 제한을 받아 바람직하지 못하다.However, considering that the plasma hydrophilization process is expensive and the electroless plating should be carried out in a wet atmosphere as a subsequent process, the process is complicated and time-limited because the process must be performed after the vacuum dry process and the wet process. Not desirable

본 발명의 목적은 상기와 같은 종래 기술의 문제점을 해결하기 위한 것으로, 균질한 두께를 가지는 니켈도금층이 구비된 탄소폼 및 이의 제조방법을 제공하는 것에 있다.An object of the present invention is to solve the problems of the prior art as described above, and to provide a carbon foam and a method for manufacturing the same with a nickel plated layer having a uniform thickness.

본 발명의 다른 목적은, 암모니아 용액에 탄소폼을 침적시켜 친수화함으로써 친수화 처리 공정이 간소화되고, 이러한 친수화 처리에 의한 니켈도금층의 형성이용이하도록 한 니켈도금층이 구비된 탄소폼 및 이의 제조방법을 제공하는 것에 있다.Another object of the present invention is to simplify the hydrophilization treatment process by depositing carbon foam in an ammonia solution to hydrophilize, and to form a nickel plated layer by the hydrophilization treatment, the carbon foam having a nickel plating layer and its preparation To provide a method.

본 발명에 의한 니켈도금층이 구비된 탄소폼은, 내부에 기공이 형성되고 친수성을 가지는 탄소폼과, 상기 기공의 내면 및 탄소폼의 외면에 코팅된 니켈도금층을 포함하여 구성됨을 특징으로 한다.Carbon foam having a nickel plating layer according to the present invention is characterized in that it comprises a carbon foam having pores formed therein and having hydrophilicity, and a nickel plating layer coated on the inner surface of the pores and the outer surface of the carbon foam.

상기 기공은 다수로 구비되며, 상기 다수 기공은 서로 연통하는 것을 특징으로 한다.The pores are provided in plurality, characterized in that the plurality of pores are in communication with each other.

상기 탄소폼은 물과 25°이하의 접촉각을 갖는 것을 특징으로 한다.The carbon foam is characterized in that it has a contact angle of less than 25 °.

본 발명에 의한 니켈도금층이 구비된 탄소폼의 제조방법은, 내부에 다수 기공이 형성된 탄소폼을 암모니아에 침적하여 친수화 처리하는 탄소폼친수화단계와, 친수화 처리된 탄소폼을 무전해도금법으로 니켈도금층을 형성하는 니켈도금층형성단계로 이루어지는 것을 특징으로 한다.The method for producing carbon foam having a nickel plating layer according to the present invention includes a carbon foam hydrophilization step of hydrophilizing a carbon foam having a plurality of pores formed therein in ammonia, and electroless plating of the hydrophilized carbon foam. Characterized in that the nickel plated layer forming step of forming a nickel plated layer.

상기 탄소폼친수화단계는, 50 내지 60℃의 암모니아 용액에 40 내지 60분간 침적시켜 친수화하는 친수화과정과, 친수화된 탄소폼의 표면을 활성화하는 활성화과정으로 이루어지는 것을 특징으로 한다.The carbon foam hydrophilization step is characterized by consisting of a hydrophilization process of hydrophilization by immersing in ammonia solution at 50 to 60 ℃ for 40 to 60 minutes, and activating the surface of the hydrophilized carbon foam.

상기 니켈도금층형성단계는, 25g/L의 NiSO4와, 50g/L의 구연산나트륨과, 25g/L의 하이포아인산염을 포함하는 도금액을 이용하여 탄소폼의 내/외면에 니켈도금층을 형성하는 과정임을 특징을 한다.The nickel plating layer forming step is a process of forming a nickel plating layer on the inner and outer surfaces of the carbon foam using a plating solution containing 25 g / L NiSO 4 , 50 g / L sodium citrate, and 25 g / L hypophosphite It is characterized by that.

상기 도금액은 9 내지 11의 pH 범위로 제한됨을 특징으로 한다.The plating liquid is characterized in that it is limited to a pH range of 9 to 11.

상기 활성화과정은, PdCl2 이 포함된 수용액 내부에 탄소폼을 침적하는 과정임을 특징으로 한다.The activation process is characterized in that the process of depositing carbon foam in an aqueous solution containing PdCl 2 .

상기 활성화과정 이후에는, 상기 탄소폼에 잔존하는 PdCl2를 제거하는 세척과정이 구비됨을 특징으로 한다.After the activation process, characterized in that the washing process for removing the PdCl 2 remaining in the carbon foam.

본 발명에 의한 니켈도금층이 구비된 탄소폼은, 균질한 두께의 니켈도금층이 구비되는 이점이 있다.Carbon foam provided with a nickel plated layer according to the present invention has the advantage that a nickel plated layer of homogeneous thickness is provided.

본 발명에 의한 니켈도금층이 구비된 탄소폼의 제조방법에서는, 암모니아 용액에 탄소폼을 침적시켜 친수화함으로써 친수화 처리 공정이 간소화되며, 이러한 친수화 처리에 의한 니켈도금층의 형성이 용이한 이점이 있다.In the method for producing a carbon foam with a nickel plated layer according to the present invention, the hydrophilization treatment process is simplified by depositing carbon foam in an ammonia solution and making it hydrophilic, and the advantage of easy formation of the nickel plating layer by such hydrophilization treatment is have.

도 1 은 본 발명에 의한 니켈도금층이 구비된 탄소폼의 단면 확대 사진.
도 2 는 본 발명에 의한 니켈도금층이 구비된 탄소폼의 제조방법을 나타낸 공정 순서도.
도 3 은 본 발명에 의한 니켈도금층이 구비된 탄소폼의 제조방법에서 일단계인 탄소폼친수화단계를 세부적으로 나타낸 공정 순서도.
도 4a 내지 도 4d 는 본 발명에 의한 니켈도금층이 구비된 탄소폼의 제조방법에서 일단계인 탄소폼친수화단계 중 암모니아 용액과의 접촉 시간 변화에 따른 물접촉각 변화를 보인 확대 사진.
도 5 는 도 4a 내지 도 4d의 실험 결과를 나타낸 그래프.
도 6 은 본 발명에 의한 니켈도금층이 구비된 탄소폼의 제조방법에서 활성화과정 실시 여부에 따른 니켈도금층의 형성 상태를 나타낸 실시예의 사진.
도 7 은 본 발명에 의한 니켈도금층이 구비된 탄소폼의 제조방법에서 일단계인 니켈도금층형성단계 중 도금액의 pH 변화에 따른 도금속도(㎛/min)변화량을 나타낸 그래프.
도 8 은 도금액의 pH 변화에 따른 인(P)의 변화량을 나타낸 그래프.
도 9 는 본 발명에 의한 니켈도금층이 구비된 탄소폼의 단면 확대 사진.1 is an enlarged cross-sectional view of a carbon foam with a nickel plating layer according to the present invention.
Figure 2 is a process flow chart showing a method for producing a carbon foam with a nickel plating layer according to the present invention.
Figure 3 is a process flowchart showing in detail the carbon foam hydrophilization step is a step in the method for producing a carbon foam with a nickel plating layer according to the present invention.
Figures 4a to 4d is an enlarged photograph showing a change in the water contact angle according to the change in contact time with the ammonia solution during the carbon foam hydrophilization step is a step in the carbon foam manufacturing method with a nickel plating layer according to the present invention.
Figure 5 is a graph showing the experimental results of Figures 4a to 4d.
Figure 6 is a photograph of an embodiment showing the state of the nickel plated layer formed according to whether the activation process in the method for producing a carbon foam with a nickel plated layer according to the present invention.
Figure 7 is a graph showing the change in plating rate (㎛ / min) according to the pH change of the plating solution during the nickel plating layer forming step of the first step in the method for producing a carbon foam with a nickel plating layer according to the present invention.
8 is a graph showing the amount of change in phosphorus (P) according to the pH change of the plating solution.
Figure 9 is an enlarged cross-sectional view of the carbon foam with nickel plated layer according to the present invention.

이하 첨부된 도 1을 참조하여 본 발명에 의한 니켈도금층을 구비한 탄소폼의 구성을 설명한다.Hereinafter, a configuration of a carbon foam having a nickel plating layer according to the present invention will be described with reference to FIG. 1.

도 1에는 본 발명에 의한 니켈도금층이 구비된 탄소폼의 확대 사진이 도시되어 있다.1 is an enlarged photograph of a carbon foam provided with a nickel plating layer according to the present invention.

첨부된 도면과 같이, 본 발명에 의한 탄소폼(10)은 내부에 다수 기공(12)이 형성되어 있으며, 상기 다수 기공(12)들은 서로 연통하도록 형성된다.As shown in the accompanying drawings, the carbon foam 10 according to the present invention is formed with a plurality of pores 12 therein, the plurality of pores 12 are formed to communicate with each other.

그리고, 서로 연통하는 다수 기공(12)의 표면에는 니켈도금층(14)이 구비된다.The nickel plating layer 14 is provided on the surface of the plurality of pores 12 communicating with each other.

상기 니켈도금층(14)은 미리 제조된 소수성 탄소폼에 친수화 처리를 실시한 후 도금액을 이용하여 형성한 것으로, 상기 탄소폼을 친수화 처리를 통해 물과 25°이하의 접촉각을 갖도록 함으로써 형성 가능하다.The nickel plated layer 14 is formed by using a plating solution after performing hydrophilization treatment on a hydrophobic carbon foam prepared in advance. The nickel plating layer 14 may be formed by having a contact angle of 25 ° or less with water through a hydrophilization treatment. .

상기 친수화 처리 및 니켈도금층(14)의 형성 방법은 아래에서 상세히 하기로 한다.The hydrophilization treatment and the method of forming the nickel plated layer 14 will be described in detail below.

이하 첨부된 도 2를 참조하여 니켈도금층(14)을 구비한 탄소폼(10)의 제조방법을 설명한다.Hereinafter, a method of manufacturing the carbon foam 10 having the nickel plated layer 14 will be described with reference to FIG. 2.

도 2에는 본 발명에 의한 니켈도금층이 구비된 탄소폼(10)의 제조방법을 나타낸 공정 순서도가 도시되어 있다.2 is a process flowchart showing a method for manufacturing a carbon foam 10 provided with a nickel plated layer according to the present invention.

도면과 같이, 니켈도금층이 구비된 탄소폼(10)을 제조하는 과정은, 내부에 다수 기공(12)이 형성된 탄소폼(도 8의 도면부호 F 참조)을 암모니아에 침적하여 친수화 처리하는 탄소폼친수화단계(S100)와, 친수화 처리된 탄소폼(F)을 무전해도금법으로 니켈도금층(14)을 형성하는 니켈도금층형성단계(S200)로 이루어지는 것을 특징으로 한다.As shown in the drawing, the process of manufacturing the carbon foam 10 provided with a nickel plating layer, the carbon foam having a plurality of pores 12 formed therein (see reference numeral F of FIG. 8) in ammonia to hydrophilize the carbon Form-form hydrophilization step (S100), and the nickel-plated layer forming step (S200) of forming a nickel plating layer 14 by electroless plating the hydrophilized carbon foam (F) is characterized in that it consists of.

상기 탄소폼(F)은 도 8과 같이, 내부에 서로 연통하는 다수의 기공(12)이 형성된 범위 내에서 다양한 제조방법에 따라 제조된 모든 탄소폼(F)이 적용 가능하다.The carbon foam (F) is applicable to all the carbon foam (F) manufactured according to various manufacturing methods within the range in which a plurality of pores 12 are formed in communication with each other, as shown in FIG.

상기 탄소폼친수화단계(S100)는, 니켈도금층형성단계(S200)를 위한 준비단계로서, 일반적인 탄소폼(F)은 소수성을 가지고 있어서 도금액을 이용한 니켈도금층(14)의 형성이 쉽지 않다.The carbon foam hydrophilization step (S100) is a preparation step for the nickel plating layer forming step (S200), the general carbon foam (F) has a hydrophobicity, it is not easy to form the nickel plating layer 14 using a plating solution.

따라서, 상기 탄소폼친수화단계(S100)를 실시하여 탄소폼(F)의 친수화를 도모하게 된다.Therefore, the carbon foam hydrophilization step (S100) is carried out to promote the hydrophilization of the carbon foam (F).

보다 구체적으로 살펴보면, 상기 탄소폼친수화단계(S100)는 도 3과 같이, 크게 탄소폼(F)의 친수화처리를 위한 친수화과정(S120)과, 친수화된 탄소폼(F)의 표면을 활성화하는 활성화과정(S140)으로 이루어진다.In more detail, the carbon foam hydrophilization step (S100), as shown in Figure 3, the hydrophilization process (S120) for the hydrophilization treatment of carbon foam (F) large, the surface of the hydrophilized carbon foam (F) Activation process is made (S140).

상기 친수화과정(S120)에서 본 발명에서는 암모니아 용액을 이용하여 실시하였다. 즉, 상기 친수화과정(S120)은 암모니아 용액에 탄소폼(F)을 침적하여 친수화 처리하였으며, 첨부된 도 4a 내지 도 4d에는 친수화과정(S120)의 실시 시간 변화에 따른 친수화 정도의 변화를 실물 사진으로 증명하였다.In the hydrophilization process (S120) in the present invention was carried out using ammonia solution. That is, the hydrophilization process (S120) was hydrophilized by depositing carbon foam (F) in the ammonia solution, the accompanying Figures 4a to 4d of the degree of hydrophilization according to the implementation time of the hydrophilization process (S120) The change was demonstrated in real photos.

첨부된 도면에서 도 4a는 친수화과정(S120)을 실시하지 않은 탄소폼(F)의 물접촉각을 나타낸 것으로, 85°를 나타내어 소수성을 가지는 것을 알 수 있었다.In the accompanying drawings, Figure 4a shows the water contact angle of the carbon foam (F) not subjected to the hydrophilization process (S120), it can be seen that the hydrophobicity represented by 85 °.

그리고, 본 발명의 실시예에서 친수화과정(S120)을 실시하되 암모니아 용액과의 접촉시간을 경과시키면서 관찰한 결과, 상기 친수화과정(S220)을 20분간 실시한 도 4b의 경우 친수화과정(S120)이 완료된 직후에는 48°의 물접촉각을 나타내었고, 친수화과정(S120) 완료 3시간 후에는 55°의 물접촉각을 나타내어 소수성을 띄고 있었다.In addition, in the embodiment of the present invention, while performing the hydrophilization process (S120) while observing while passing the contact time with the ammonia solution, the hydrophilization process (S220) in the case of FIG. The water contact angle of 48 ° was shown immediately after the completion of), and the water contact angle of 55 ° was shown after 3 hours of hydrophilization (S120).

그러나, 도 4c와 같이 친수화과정(S120)을 40분간 실시한 직후 24°의 물접촉각을 나타내어 친수성을 나타내었다.However, after performing the hydrophilization process (S120) for 40 minutes as shown in FIG. 4C, the water contact angle of 24 ° was shown to indicate hydrophilicity.

그리고, 상기 친수화과정(S120)을 보다 연장하여 60분간 실시한 직후에는 15°의 물접촉각을 나타내었고, 60분간의 친수화과정(S120)을 완료한 후 3시간이 경과하였을 때에는 도 4d와 같이 40°의 물접촉각을 나타내었다.And, after extending the hydrophilization process (S120) for more than 60 minutes, the water contact angle was 15 °, and after 3 hours of completion of the 60-minute hydrophilization process (S120), as shown in FIG. 4D. A water contact angle of 40 ° is shown.

상기한 바와 같이 친수화과정(S120)을 마친 탄소폼(F)은 대기 중에 방치함에 따라 탄소폼(F)의 표면에 일시적으로 형성되어 있던 NH기가 소멸되기 시작하여 물접촉각이 다소 증가하는 결과를 보였다.As described above, the carbon foam (F) that has completed the hydrophilization process (S120) begins to disappear as the NH group temporarily formed on the surface of the carbon foam (F) as it is left in the air results in a slight increase in water contact angle. Seemed.

따라서, 상기 친수화과정(S120)은 40 내지 60분간 실시됨이 바람직하며, 상기 친수화과정(S120)이 완료되면 빠른 시간(적어도 3시간) 내에 후 공정을 실시함이 바람직하다.Therefore, the hydrophilization process (S120) is preferably carried out for 40 to 60 minutes, and when the hydrophilization process (S120) is completed, it is preferable to perform a post-process within a short time (at least 3 hours).

본 발명의 실시예에서 암모니아 용액은 60℃로 유지하고 9 ~ 11 의 pH 범위 내에서 실시하였다.In the embodiment of the present invention, the ammonia solution was maintained at 60 ° C and carried out within a pH range of 9-11.

첨부된 도 5는 도 4a 내지 도 4d의 실험 결과를 정리한 그래프이다.5 is a graph summarizing the experimental results of FIGS. 4A to 4D.

상기 친수화과정(S120) 이후에는 활성화과정(S140)이 실시된다. 상기 활성화과정(S140)은, 비금속인 탄소폼(F)에 무전해도금법을 이용하여 니켈도금층(14)을 형성하기 위해 요구되는 공정이다.After the hydrophilization process (S120), the activation process (S140) is carried out. The activation process (S140) is a process required for forming the nickel plated layer 14 on the non-metal carbon foam (F) by using an electroless plating method.

본 발명의 실시예에서는, SnCl2 10g 을 HCl 30㎖에 투입한 후 증류수를 추가하여 총 1ℓ가 되도록 한 용액에 탄소폼(10)을 상온 침적한 후, PdCl2 용액에 다시 침적함으로써 완료된다.In an embodiment of the present invention, 10 g of SnCl 2 was added to 30 mL of HCl, and carbon dioxide (10) was then deposited at room temperature in a solution prepared by adding distilled water to a total of 1 L, followed by PdCl 2 Complete by submersion in solution again.

도 6에는 본 발명에 의한 니켈도금층이 구비된 탄소폼의 제조방법에서 활성화과정 실시 여부에 따른 니켈도금층의 형성 상태를 나타낸 실시예의 사진이 도시되어 있다.Figure 6 is a photograph of an embodiment showing a state of forming a nickel plating layer according to whether or not the activation process in the method for producing a carbon foam with a nickel plating layer according to the present invention.

첨부된 도 6에서 (a)는 활성화처리를 하지 않은 탄소폼(F)으로 니켈도금층형성단계(S300)를 실시한 경우로서, 니켈도금층(14)이 전혀 형성되어 있지 않은 것을 확인할 수 있다.In FIG. 6 (a), when the nickel plating layer forming step S300 is performed with the carbon foam F not activated, it may be confirmed that the nickel plating layer 14 is not formed at all.

반면, 도 6의 (b)는 PdCl2 가 포함된 수용액을 이용하여 탄소폼(F)에 활성화과정(S140)을 실시한 경우에는 니켈도금층(14)이 고르게 형성되어 있음을 확인할 수 있다. On the other hand, Figure 6 (b) it can be seen that the nickel plating layer 14 is evenly formed when the activation process (S140) to the carbon foam (F) using an aqueous solution containing PdCl 2 .

상기와 같은 과정에 따라 활성화과정(S140)이 완료되면, 세척과정(S160)이 실시된다. 상기 세척과정(S160)은 탄소폼(F)의 표면에 잔존하는 PdCl2 를 제거하기 위한 과정으로, 본 발명의 실시예에서는 증류수를 사용하였다.When the activation process (S140) is completed according to the above process, the washing process (S160) is carried out. The washing process (S160) is a process for removing PdCl 2 remaining on the surface of the carbon foam (F), distilled water was used in the embodiment of the present invention.

상기 탄소폼친수화단계(S100) 이후에는 상기 니켈도금층형성단계(S200)가 실시된다. 상기 니켈도금층형성단계(S200)는, 탄소폼친수화단계(S200)에서 친수화 및 활성화된 탄소폼(F)의 내/외부에 니켈도금층(14)을 형성하는 과정으로서, 상기 기공(12)의 내부 표면과 탄소폼(F)의 외면에 균일한 니켈도금층(14)이 형성되도록 한다.After the carbon foam hydrophilization step (S100), the nickel plating layer forming step (S200) is performed. The nickel plating layer forming step (S200) is a process of forming the nickel plating layer 14 inside / outside of the hydrophilized and activated carbon foam (F) in the carbon foam hydrophilization step (S200). The uniform nickel plating layer 14 is formed on the inner surface and the outer surface of the carbon foam (F).

상기 니켈도금층형성단계(S200)에서 니켈도금층(14)을 형성하기 위한 도금액은, 25g/L의 NiSO4와, 50g/L의 구연산나트륨과, 25g/L의 하이포아인산염을 포함하도록 구성하였으며, 9 내지 11의 pH 범위로 제한하였다.In the nickel plating layer forming step (S200), the plating liquid for forming the nickel plating layer 14 was configured to include 25 g / L NiSO 4 , 50 g / L sodium citrate, and 25 g / L hypophosphite, Limited to a pH range of 9-11.

pH를 9, 10, 11로 변화시켜 20분간 무전해 도금을 실시한 후 두께를 측정한 결과, 첨부된 도 7과 같이 pH가 증가할수록 니켈도금층(14)의 두께가 증가하였으며, 첨부된 도 8과 같이 인(P)의 양은 감소하는 것을 알 수 있다.The thickness was measured after electroless plating for 20 minutes by changing the pH to 9, 10, and 11, and as the pH was increased as shown in FIG. 7, the thickness of the nickel plated layer 14 was increased. As can be seen the amount of phosphorus (P) decreases.

그리고, 이러한 결과에 따라 도금액의 pH 를 조절함으로써 니켈도금층(14)의 두께 조절이 가능할 것으로 판단된다.In addition, it is determined that the thickness of the nickel plated layer 14 may be adjusted by adjusting the pH of the plating liquid according to the result.

상기와 같은 과정에 따라 제조된 니켈도금층이 구비된 탄소폼(10)은 첨부된 도 9와 같다.Carbon foam 10 provided with a nickel plated layer prepared according to the above process is as shown in FIG.

즉, 도 9는 본 발명에 의한 니켈도금층(14)이 구비된 탄소폼(10)의 단면 확대 사진으로서, 탄소폼(10) 내부에 수 ~ 수십㎛ 크기를 가지는 기공(12)이 다수 형성되어 있고, 상기 기공(12) 내부 표면에 니켈도금층(14)이 고르게 형성되어 상기 기공(12)과 탄소폼(F)이 니켈도금층(14)에 의해 구획되어 있음을 확인할 수 있다.
그리고, 상기 니켈도금층(14)은 기공(12)의 내부가 탄소폼(F)의 외부로 개구되도록(도 9에서 볼 때 전/후 방향) 형성된다.That is, FIG. 9 is an enlarged cross-sectional view of the carbon foam 10 having the nickel plating layer 14 according to the present invention, and a plurality of pores 12 having a size of several tens of micrometers are formed in the carbon foam 10. The nickel plating layer 14 is evenly formed on the inner surface of the pores 12, so that the pores 12 and the carbon foam F are partitioned by the nickel plating layer 14.
In addition, the nickel plating layer 14 is formed such that the inside of the pores 12 is opened to the outside of the carbon foam F (front / rear direction in FIG. 9).

이러한 본 발명의 범위는 상기에서 예시한 실시예에 한정되지 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-described embodiments, and many other modifications based on the present invention will be possible to those skilled in the art within the scope of the present invention.

10. 니켈도금층이 구비된 탄소폼 12. 기공
14. 니켈도금층 F . 탄소폼
S100. 탄소폼친수화단계 S120. 친수화과정
S140. 활성화과정 S160. 세척과정
S200. 니켈도금층형성단계10. Carbon foam with nickel plated layer 12. Pore
14. Nickel plated layer F. Carbon foam
S100. Carbon foam hydrophilization step S120. Hydrophilization Process
S140. Activation process S160. Washing process
S200. Nickel Plating Layer Formation Step

Claims (9)

서로 연통하면서 수 ~ 수십㎛의 크기를 가지는 다수 기공이 형성되고, 암모니아에 침적하여 친수처리되며, SnCl2가 투입된 HCl에 증류수를 추가한 용액에 침적한 후, PdCl2 용액에 침적되어 친수성을 가지는 탄소폼과,
상기 다수 기공의 내부면 및 탄소폼의 표면에 무전해도금법으로 코팅된 니켈도금층을 포함하여 구성됨을 특징으로 하는 니켈도금층이 구비된 탄소폼.A plurality pores having a size in number to several tens ㎛ and communicate with each other is formed, and immersed in ammonia is treated hydrophilic, SnCl After 2 deposited on the injected solution was added distilled water to HCl, it is immersed in PdCl 2 solution having a hydrophilic Carbon foam,
Carbon foam having a nickel plating layer, characterized in that it comprises a nickel plating layer coated on the inner surface of the plurality of pores and the surface of the carbon foam by an electroless plating method. 제 1 항에 있어서, 상기 친수처리된 탄소폼은 물과 25°이하의 접촉각을 갖는 것을 특징으로 하는 니켈도금층이 구비된 탄소폼.[Claim 2] The carbon foam having a nickel plating layer according to claim 1, wherein the hydrophilic carbon foam has a contact angle of 25 ° or less with water. 제 2 항에 있어서, 상기 니켈도금층은 탄소폼과 기공을 구획하는 것을 특징으로 하는 니켈도금층이 구비된 탄소폼.According to claim 2, wherein the nickel plating layer is carbon foam with a nickel plating layer, characterized in that the carbon foam and pores partition. 서로 연통하면서 수 ~ 수십㎛의 크기를 가지는 다수 기공이 형성된 탄소폼을 50 내지 60℃의 암모니아 용액에 40 내지 60분간 침적하여 친수화 처리하는 친수화과정과, 상기 친수화처리된 탄소폼을 SnCl2가 투입된 HCl에 증류수를 추가한 용액에 침적한 후, PdCl2 용액에 침적하여 활성화하는 활성화과정과, 활성화된 탄소품에 잔존하는 PdCl2 를 증류수로 제거하는 세척과정으로 이루어진 탄소폼친수화단계와; 상기 탄소폼친수화단계를 거친 탄소폼에 무전해도금법을 실시하여 상기 다수 기공의 내부면 및 탄소폼의 표면에 니켈도금층을 형성하는 니켈도금층형성단계로 이루어지는 것을 특징으로 하는 니켈도금층이 구비된 탄소폼의 제조방법.The hydrophilization process of immersing carbon foam having a plurality of pores having a size of several to several tens of micrometers while being in communication with each other in ammonia solution at 50 to 60 ° C. for 40 to 60 minutes to hydrophilize and SnCl the hydrophilized carbon foam 2 is immersed in a solution in which distilled water is added to HCl added thereto, followed by activating by immersing in PdCl 2 solution, and washing with PdCl 2 in the activated carbon product to remove distilled water. ; Carbon foam having a nickel plating layer, comprising a nickel plating layer forming step of performing an electroless plating method on the carbon foam subjected to the carbon foam hydrophilization step to form a nickel plating layer on the inner surface of the plurality of pores and the surface of the carbon foam. Manufacturing method. 제 4 항에 있어서, 상기 니켈도금층형성단계는,
상기 다수 기공의 내부가 개방된 상태를 유지하도록 니켈도금층을 형성하는 과정임을 특징으로 하는 니켈도금층이 구비된 탄소폼의 제조방법.The method of claim 4, wherein the nickel plating layer forming step,
Method for producing a carbon foam with a nickel plating layer, characterized in that the process of forming a nickel plating layer to maintain the interior of the plurality of pores open. 제 5 항에 있어서, 상기 니켈도금층형성단계는,
25g/L의 NiSO4와, 50g/L의 구연산나트륨과, 25g/L의 하이포아인산염을 포함하는 도금액을 이용하여 탄소폼의 내/외면에 니켈도금층을 형성하는 과정임을 특징을 하는 니켈도금층이 구비된 탄소폼의 제조방법.The method of claim 5, wherein the nickel plating layer forming step,
The nickel plating layer is a process of forming a nickel plating layer on the inner and outer surfaces of carbon foam using a plating solution containing 25 g / L NiSO 4 , 50 g / L sodium citrate, and 25 g / L hypophosphite. Method for producing a carbon foam provided. 제 6 항에 있어서, 상기 도금액은 9 내지 11의 pH 범위로 제한됨을 특징으로 하는 니켈도금층이 구비된 탄소폼의 제조방법.7. The method of claim 6, wherein the plating solution is limited to a pH range of 9 to 11. 제 7 항에 있어서, 상기 활성화과정은,
상기 친수화과정 완료 후 3시간 이내에 실시됨을 특징으로 하는 니켈도금층이 구비된 탄소폼의 제조방법.The method of claim 7, wherein the activation process,
Method of producing a carbon foam with a nickel plating layer, characterized in that performed within 3 hours after the completion of the hydrophilization process. 삭제delete
KR1020100042958A 2010-05-07 2010-05-07 The carbon foam having a nickel coating layer and method for manufacturing same KR101156509B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
KR1020100042958A KR101156509B1 (en) 2010-05-07 2010-05-07 The carbon foam having a nickel coating layer and method for manufacturing same

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
KR1020100042958A KR101156509B1 (en) 2010-05-07 2010-05-07 The carbon foam having a nickel coating layer and method for manufacturing same

Publications (2)

Publication Number Publication Date
KR20110123460A KR20110123460A (en) 2011-11-15
KR101156509B1 true KR101156509B1 (en) 2012-06-18

Family

ID=45393622

Family Applications (1)

Application Number Title Priority Date Filing Date
KR1020100042958A KR101156509B1 (en) 2010-05-07 2010-05-07 The carbon foam having a nickel coating layer and method for manufacturing same

Country Status (1)

Country Link
KR (1) KR101156509B1 (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101183029B1 (en) * 2012-04-03 2012-09-14 한국기계연구원 Method for manufacturing metal infiltration casting product using porous carbon preform and the metal infiltration casting product using thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060133012A (en) * 2004-03-15 2006-12-22 캐보트 코포레이션 Modified carbon products and their applications
KR20080112234A (en) * 2006-02-15 2008-12-24 루디야드 라일 이스트반 Mesoporous activated carbon

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060133012A (en) * 2004-03-15 2006-12-22 캐보트 코포레이션 Modified carbon products and their applications
KR20080112234A (en) * 2006-02-15 2008-12-24 루디야드 라일 이스트반 Mesoporous activated carbon

Also Published As

Publication number Publication date
KR20110123460A (en) 2011-11-15

Similar Documents

Publication Publication Date Title
JP3101922B2 (en) Method for producing metal foam and obtained metal foam
Rebbecchi Jr et al. Template-based fabrication of nanoporous metals
KR101175232B1 (en) Current collector-electrode one body type device and manufacturing method thereof
CN101649477B (en) Preparation method of metal carbon aerogel composite material
JPS62155937A (en) Production of catalytic body carrying gold and gold composite oxide
WO2009070574A2 (en) Methods for modification of polymers, fibers and textile media
CN113015589B (en) Metal foam body and method for producing same
US4916110A (en) Microporous catalytic material and support structure
JP3905939B2 (en) POROUS STRUCTURE HAVING PREMETALLIZED CONDUCTIVE POLYMER COATING AND PROCESS FOR PRODUCING THE SAME
KR101156509B1 (en) The carbon foam having a nickel coating layer and method for manufacturing same
US20170292189A1 (en) Porous Materials
EP1899157B1 (en) Method of fabricating nanoscale structures
KR101329104B1 (en) Manufacturing method of rayon -type activated carbon fiber using potassium permanganate
CN108660489B (en) Preparation method of three-dimensional porous metal material with non-deviation aperture and physical property
JP6899692B2 (en) Method for producing catalyst for hydrogen production
CN100357027C (en) Metal carrier for automobile tail gas purifier catalyst and its prepn
KR20200127966A (en) Method for manufacturing an open pore molded article made of metal and a molded article manufactured using the method
CN110724941B (en) Method for preparing porous metal film by chemical plating process
CN102162094B (en) Cyclic chemical plating process for preparing palladium or palladium alloy membrane
KR940002752B1 (en) Method for preparing metal fiber articles
KR100763259B1 (en) Lead-coated composite porous structures and corresponding conductive activation methods
JP3735898B2 (en) Method for producing porous metal body
KR100531130B1 (en) Preparation of composite palladium membranes using etching process of metal chlorides
CN118724571B (en) Preparation method of porous ceramic and porous ceramic
CN110639485A (en) Preparation of supported TiO by distributed deposition method2Method for preparing photocatalyst

Legal Events

Date Code Title Description
A201 Request for examination
PA0109 Patent application

Patent event code: PA01091R01D

Comment text: Patent Application

Patent event date: 20100507

PA0201 Request for examination
E902 Notification of reason for refusal
PE0902 Notice of grounds for rejection

Comment text: Notification of reason for refusal

Patent event date: 20111020

Patent event code: PE09021S01D

PG1501 Laying open of application
E701 Decision to grant or registration of patent right
PE0701 Decision of registration

Patent event code: PE07011S01D

Comment text: Decision to Grant Registration

Patent event date: 20120521

GRNT Written decision to grant
PR0701 Registration of establishment

Comment text: Registration of Establishment

Patent event date: 20120608

Patent event code: PR07011E01D

PR1002 Payment of registration fee

Payment date: 20120611

End annual number: 3

Start annual number: 1

PG1601 Publication of registration
FPAY Annual fee payment

Payment date: 20160308

Year of fee payment: 5

PR1001 Payment of annual fee

Payment date: 20160308

Start annual number: 5

End annual number: 5

FPAY Annual fee payment

Payment date: 20170308

Year of fee payment: 6

PR1001 Payment of annual fee

Payment date: 20170308

Start annual number: 6

End annual number: 6

FPAY Annual fee payment

Payment date: 20190311

Year of fee payment: 8

PR1001 Payment of annual fee

Payment date: 20190311

Start annual number: 8

End annual number: 8

FPAY Annual fee payment

Payment date: 20200309

Year of fee payment: 9

PR1001 Payment of annual fee

Payment date: 20200309

Start annual number: 9

End annual number: 9

PC1903 Unpaid annual fee

Termination category: Default of registration fee

Termination date: 20220319