KR950704542A - 나노결정성 금속(nanocrystalline metals) - Google Patents

나노결정성 금속(nanocrystalline metals) Download PDF

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KR950704542A
KR950704542A KR1019950702133A KR19950702133A KR950704542A KR 950704542 A KR950704542 A KR 950704542A KR 1019950702133 A KR1019950702133 A KR 1019950702133A KR 19950702133 A KR19950702133 A KR 19950702133A KR 950704542 A KR950704542 A KR 950704542A
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nanocrystalline
milliseconds
metal material
cathode
nickel
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에르브 우웨
엠. 엘-셰릭 압델모우남
케이. 에스. 청 세드릭
제이. 아우스 마틴
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수잔 포르티에, 앨리슨 모건
퀸′즈 유니버시티 앳 킹스턴
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    • 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
    • C25D5/18—Electroplating using modulated, pulsed or reversing current
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y25/00—Nanomagnetism, e.g. magnetoimpedance, anisotropic magnetoresistance, giant magnetoresistance or tunneling magnetoresistance
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
    • 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
    • C25D5/60—Electroplating characterised by the structure or texture of the layers
    • C25D5/615—Microstructure of the layers, e.g. mixed structure
    • C25D5/617—Crystalline layers
    • 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
    • C25D5/60—Electroplating characterised by the structure or texture of the layers
    • C25D5/623—Porosity of the layers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S75/00—Specialized metallurgical processes, compositions for use therein, consolidated metal powder compositions, and loose metal particulate mixtures
    • Y10S75/954—Producing flakes or crystals

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Nanotechnology (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Inorganic Insulating Materials (AREA)
  • Catalysts (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)
  • Glass Compositions (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

나노결정성 소재, 특히, 평균 압도가 약11나노미터 미만인 나노 결정성 니켈 및 NiFeCr 및 NiFeCrMn 합금과 같이 입도가 약100nm 미만인 3원 및 4원 니켈-철 합금을 제조하는 방법이 설명된다. 나노결정성 니켈은 펄스 D.C. 전류의 인가에 의해 수성 산성 전해조 중에서 음극 상에 전기 증착된다. 3원 및 4원 니켈-철 합금과 기타 2원, 3원 및 4원 합금은 D.C. 전기도금 또는 펄스 D.C. 전기도금에 의해 제조될 수 있다. 전해조내의 전해질은 또한 입도조절을 보조하는 사카린과 같은 스트레스 완화제를 함유한다. 본 발명의 신규한 생성물은 내마모성 코팅물, 수소저장 소재, 자성 소재 및 수소 발생을 위한 촉매로서 사용될 수 있다.

Description

나노결정성 금속(NANOCRYSTALLINE METALS)
본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음
제1도는 본 발명의 방법에서 사용되는 장치의 한가지 구체예의 다이아그램적인 스케치임,
제5도는 본 발명에서 사용된 장치의 또 다른 구체예를 나타낸 다이아그램적인 스케치임.

Claims (27)

  1. 다음 단계로 이루어짐을 특징으로 하는, 기판 상에 선택된 금속 소재를 나노결정성 형태로 전기 증착시키는 방법 : (a)양극과 음극을 갖는 전해조를 준비하고 ; (b)선택된 금속 소재의 이온을 함유하는 수성, 전해질을 상기 전해조에 도입한 다음 ; (c)상기 전해질을 약15 내지 약 75℃의 온도범위에서 유지시키고; (d)피크전류밀도가 약 0.1 내지 약 30A/㎠ 범위인 DC전류를 양극과 음극 사이에서 약 0.1 내지 5밀리초의 기간동안 흘려 보내고 약 1내지 500밀리초 동안은 통과하지 않도록 펄스 간격을 두고 전류를 통과시켜 상기 선택된 금속 소재를 상기 음극 상에 나노결정성 형태로 증착시킨다.
  2. 제1항에 있어서, 상기 선택된 금속 소재가 (a)Co, Cr, Cu 및 Fe 중에서 선택된 순수한 금속 또는 (b)Ni, Fe, co, Zn, w, Cr, Cu, Mo, Mn, V, Si, P, C, 및 S중에서 선택된 두 가지 이상의 원소를 함유하는 합금(단, 상기 제1원소가 니켈인 2원 합금인 경우, 제2원소는 철 또는 인이 아니고, 상기 제1원소가 Co인 2원 합금에서는, 제2원소는 W가 아님) 중에서 선택된, 100㎜ 미만의 입도를 갖는 나노 결정성 금속 소재인 방법.
  3. 다음 단계로 이루어짐을 특징으로 하는 선택된 금속 소재를 나노결정성 형태로 전기 증착시키는 방법:(a)양극과 음극을 갖는 전해조를 준비하고; (b)선택된 금속 소재의 이온을 함유하는 수성, 산성 전해질을 상기 전해조에 도입한 다음; (c) 상기 전해질을 약55내지 약75℃의 온도범위에서 유지시키고; (d)피크 전류밀도가 약 0.1 내지 약 3.0 A/㎠범위인 DC전류를 양극과 음극사이에서 약 1.0 내지 5밀리초의 기간동안 흘려 보내고 약 30 내지 5밀리초 동안은 통과하지 않도록 펄스 간격을 두고 전류를 통과시켜 상기 선택된 금속 소재를 상기 음극 상에 나노결정성 형태로 증착시킨다.
  4. 제3항에 있어서, 상기 선택된 금속 소재가 니켈인 방법.
  5. 제3항에 있어서, 상기 양극이 니켈, 백금 및 흑연 중에서 선택되는 방법.
  6. 제5항에 있어서, 상기 음극이 티타늄, 강철, 황동, 구리, 니켈, 및 흑연 중에서 선택되는 방법.
  7. 제6항에 있어서, 상기 전해질이 스트레스 완화제와 입자 정제제를 약 10g/1까지 추가로 함유하는 방법.
  8. 제7항에 있어서, 상기 스트레스 완화제와 입자정제제가 사카린, 쿠마린, 소듐 라우실 설페이트 및 티오우레아 중에서 선택되는 방법.
  9. 제8항에 있어서, 상기 전해질이 입도 억제제를 추가로 함유하는 방법.
  10. 제9항에 있어서, 상기 입도 억제제가 인산인 방법.
  11. 제3항에 있어서, 상기 전류가 1.5밀리초 내지 3.0 밀리초 사이의 기간동안 흐르고 40 밀리초 내지 50 밀리초의 기간동안은 흐르지 않는 방법.
  12. 제1항에 있어서, 주기적인 펄스 역전 단계를 포함하는 방법.
  13. 제11항에 있어서, 상기 전해조가 60 내지 70℃의 온도범위에서 유지되는 방법.
  14. 제12항에 있어서, 상기 전류가 2.5밀리초 동안 통과되고 45밀리초 동안 통과되지 않는 방법.
  15. 제13항에 있어서, 상기 전해조가 65℃의 온도에서 유지되는 방법.
  16. 제11항에 있어서, 상기 피크 전류 밀도가 1.5 - 22A/㎠범위에 드는 방법.
  17. 제16항에 있어서, 상기 피크 전류 밀도가 약 1.9A/㎠인 방법.
  18. 입도가 8내지 10nm인 범위에서 최대의 경도를 갖고 통상적인 결정성 형태의 니켈 소재의 포화 자기 특성과 실제로 동등한 포화 자기 특성을 가지며, 평균 입경이 11 나노미터 미만인 나노결정성 니켈 소재.
  19. 제3항의 방법에 따라 제조되는 나노결정성 니켈.
  20. (a)Co, Cr, Cu 및 Fe 중에서 선택된 순수한 금속 및 (b)Ni, Fe, Co, Zn, Ti, Mg, w, Cr, Cu, Mo, Mn, V, Si, P, C, 및 S중에서 선택된 두가지 원소를 함유하는 합금(단, 상기 제1원소가 니켈인 2원 합금인 경우, 제2원소는 철 또는 인이 아니고, 상기 제1원소가 Co인 2원 합금에서는, 제2원소는 W가 아님) 중에서 선택된, 100nm 미만의 입도를 갖는 나노결정성 금속 소재.
  21. NiFeX1X2타입의 나노결정성이 3원 또는 4원 니켈-철 합금(식중, X1과 X2는 같거나 다르며 Cr, Co, Cu, Mo, Mn, V, Ti, Mg, Si, P, C 및 S중에서 선택된다).
  22. 제21항에 있어서, X1과 X2가 Cr 및 Mn 중에서 선택되는 나노 결정성 합금.
  23. 제21항에 있어서, X1과 X2가 Cr 및 Mo 중에서 선택되는 나노 결정성 합금.
  24. 제21항에 있어서, X1과 X2가 Mo 및 Mn 중에서 선택되는 나노 결정성 합금.
  25. 제21항에 있어서, X1과 X2가 Cu 및 Cr 중에서 선택되는 나노 결정성 합금.
  26. 제1항에 있어서, 상기 전해질이 사카린, 소듐 시트레이트, EDTA, 구연산, 소듐 플루오라이드, 쿠마린, 소듐 라우릴 설페이트 및 타오우레아 중에서 선택된 입자 정제제와 스트레스 완화제를 10g/1까지 포함하는 방법.
  27. 제3항에 있어서, 주기적인 펄스 역전단계를 포함하는 방법.
    ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.
KR1019950702133A 1992-11-30 1993-11-26 나노결정성금속 KR100304380B1 (ko)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US07/983,205 US5352266A (en) 1992-11-30 1992-11-30 Nanocrystalline metals and process of producing the same
US07/983205 1992-11-30
PCT/CA1993/000492 WO1994012695A1 (en) 1992-11-30 1993-11-26 Nanocrystalline metals

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KR950704542A true KR950704542A (ko) 1995-11-20
KR100304380B1 KR100304380B1 (ko) 2001-11-22

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US (1) US5352266A (ko)
EP (1) EP0670916B2 (ko)
JP (1) JPH08503522A (ko)
KR (1) KR100304380B1 (ko)
AT (1) ATE157407T1 (ko)
BR (1) BR9307527A (ko)
CA (1) CA2148215C (ko)
DE (1) DE69313460T3 (ko)
DK (1) DK0670916T4 (ko)
ES (1) ES2108965T5 (ko)
HK (1) HK1011388A1 (ko)
SG (1) SG49720A1 (ko)
WO (1) WO1994012695A1 (ko)

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ATE157407T1 (de) 1997-09-15
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CA2148215A1 (en) 1994-06-09
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ES2108965T5 (es) 2003-09-16
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