WO2001031085A2 - Electrodes en metal amorphe/verre metallique pour procedes electrochimiques - Google Patents

Electrodes en metal amorphe/verre metallique pour procedes electrochimiques Download PDF

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Publication number
WO2001031085A2
WO2001031085A2 PCT/CA2000/001251 CA0001251W WO0131085A2 WO 2001031085 A2 WO2001031085 A2 WO 2001031085A2 CA 0001251 W CA0001251 W CA 0001251W WO 0131085 A2 WO0131085 A2 WO 0131085A2
Authority
WO
WIPO (PCT)
Prior art keywords
metallic glass
electrode
electrodes
hydrogen
amorphous
Prior art date
Application number
PCT/CA2000/001251
Other languages
English (en)
Other versions
WO2001031085A3 (fr
Inventor
Steven J. Thorpe
Donald W. Kirk
Original Assignee
Stuart Energy Systems Corporation
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 Stuart Energy Systems Corporation filed Critical Stuart Energy Systems Corporation
Priority to JP2001533216A priority Critical patent/JP2003513170A/ja
Priority to BR0014994-2A priority patent/BR0014994A/pt
Priority to EP00971182A priority patent/EP1230412A2/fr
Priority to MXPA02002673A priority patent/MXPA02002673A/es
Priority to KR1020027004542A priority patent/KR20020037772A/ko
Priority to AU10135/01A priority patent/AU1013501A/en
Publication of WO2001031085A2 publication Critical patent/WO2001031085A2/fr
Publication of WO2001031085A3 publication Critical patent/WO2001031085A3/fr
Priority to NO20020957A priority patent/NO20020957L/no

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/8605—Porous electrodes
    • H01M4/8621—Porous electrodes containing only metallic or ceramic material, e.g. made by sintering or sputtering
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/003—Making ferrous alloys making amorphous alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C45/00—Amorphous alloys
    • C22C45/04—Amorphous alloys with nickel or cobalt as the major constituent
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
    • C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
    • C25B11/061—Metal or alloy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

Definitions

  • the invention provides in one aspect a metallic glass of use in electrochemical processes, said metallic glass consisting essentially of a material of the general nominal composition
  • the electrodes have excellent thermal stability, improved stability in an aqueous electrolyte and can provide improved current efficiency - anodic or cathodic ove ⁇ otential performance. They are of use in the electrolysis of aqueous electrolyte solutions such as mixtures of caustic (KOH, NaOH) and water in the production of oxygen and hydrogen.
  • the electrodes are comprised of low cost transition metals in combination with metalloid elements in specific ratios to permit the alloy composition to be solidified into an amorphous state. They offer improved current efficiencies via anodic or cathodic ove ⁇ otential performance and offer improved stability in both static and cyclic exposures. They can be used in concentrated alkaline solutions and at elevated temperatures for improved electrode performance.
  • the electrodes are of use in the electrolysis of alkaline solutions resulting in the production of hydrogen and oxygen via the decomposition of water, and also additional uses in electrodes for fuel cells, electro-organic synthesis or environmental waste treatment.
  • Fig. 4 is a schematic diagram of a three component cell used in the evaluation of the electrochemical activity and stability of the materials according to the invention.
  • Fig. 5 is a diagrammatic representation of the apparatus of use in obtaining electrochemical measurements, and wherein the same numeral denotes like parts.
  • This Example illustrates the preparation electrodes having a nominal composition:
  • Induction heater unit 12 was comprised of an induction heater coil 28 (Fig. 2) in vacuum chamber 14, a 3-stage step-up transformer and a closed-loop water recirculator (not shown) which supplied cooling water through the induction coil during heating.
  • Fig. 2 shows the arrangement of a copper wheel 30 (20 cm in diameter, 3.8 cm in width), ceramic crucible 22 induction coil 28 in high vacuum chamber 14 and ribbon guide 32.
  • Planar amo ⁇ hous ribbons were formed on the surface of the wheel rotating counterclockwise and driven along the ribbon guides to the collector tube. This particular form of melt spinning is referred to as the planar flow casting technique. From the wheel rotation speed, a quenching rate was estimated to be ca 10° °C/sec. One side of the ribbon was free from contact with the wheel and had a shiny appearance (shiny side) compared with the dull appearance for the other side in contact with the wheel (wheel side). To minimize surface imperfections on the dull side due to contact with the wheel, the peripheral surface of the wheel was thoroughly polished with diamond paste and degreased with acetone before each run. Standard experimental parameters of the melt-spinning operation are summarized in Table 3.
  • the first evaluation relates to the actual composition of the alloys produced as poor recoveries during melting can produce substantial deviations between the nominal and actual composition of a given alloy.
  • the second evaluation relates to the structure of the alloys produced as the processing method produces a metastable structure that is amorphous or nanocrystalline in nature.
  • the third evaluation relates to the electrode performance in relation to the overvoltage necessary for hydrogen production for as-melt spun ribbons under conditions related to the electrolysis of an alkaline solution.
  • the fourth evaluation refers to the examination of the surface of the electrode materials used under both constant potential and conditions of potential cycling as described above.
  • the second test was performed using the technique of X-ray diffraction in order to confirm the degree of crystallinity of the manufactured ribbons.
  • measurements were also carried out on crystallized fragments of the amorphous alloys as well as pure elemental nickel, cobalt, chromium, boron and the intermetallic nickel boride.
  • the amorphous samples were prepared by cutting ribbons into 4 mm x 10 mm rectangular pieces. The samples were then degreased with acetone, methanol and deionized water in sequence.
  • the crystallized fragments had the same bulk composition as the corresponding amorphous alloy and were primarily in the form of brittle plate-like powder.
  • the crystallized amo ⁇ hous alloy was ground to form a fine powder in an agate mortar and dispersed on a slide glass before measurement.
  • Diffraction patterns were measured on a Siemens D5000 X-ray diffractometer using 50 kV Cu-K ⁇ radiation with a Ni filter in the range of 20 to 70 degree-2 ⁇ at a scan rate of 2 degree-2 ⁇ per minute. The data was processed by Diffrac AT software.
  • the electrolytic cell shown in Fig. 4 generally as 40 had a three- compartment structure consisting of a 300 ml capacity main body formed of Teflon containing a working electrode 42 of the ribbon of alloy of the invention, a 1/2" Teflon ® tube 44 housing a counter electrode 46, and a 1/4" Teflon ® PTFE tube filled with mercury-mercuric oxide paste (Hg/HgO) 48.
  • the compartments were separated by electrolyte-permeable membranes 50 in the form of a diaphragm or frit.
  • the counter electrode 46 was a 25 mm x 12.5 mm platinum gauze with a surface area of ca. 4.4 cm .
  • HA-501G with a 200 MHz Pentium II personal computer 60, through a GPIB interface 62 and arbitrary function generator (Hokuto Denko HA-105B) 66.
  • the fourth test was performed on amorphous alloy and crystalline surfaces to compare the degree of surface roughening and hence electrode degradation by using optical and scanning electron microscopy prior to and post use as an electrocatalyst in the cell.
  • Optical investigation was achieved using a light stereoscope and light metallograph. Electron imaging was accomplished using a
  • the structure of the ribbon was assessed using x- ray diffraction, as it is an integral part of the electrode performance independent of the exact composition of the electrode material. It is known that a typical X-ray diffraction (XRD) pattern of an amo ⁇ hous material is a broad spectrum with no prominent sha ⁇ peaks relating to crystalline structure. Thus, qualitative confirmation of the amorphous nature of an alloy is demonstrated by a broad band peak in its XRD profile.
  • XRD X-ray diffraction
  • an index viz. effective crystallite dimension was calculated to evaluate the largest potential size of crystal embryos in the melt-spun ribbons.
  • the effective crystallite dimension is expressed by the equation:
  • D Q.91 ⁇ ⁇ cos ⁇ where D is the effective crystallite dimension in nm and ⁇ is wavelength of the Cu-
  • ⁇ denotes the full width of a given diffraction peak in radians at half the maximum intensity, ⁇ is the Bragg angle of the peak maximum.
  • the effective crystallite dimension was measured for all the melt-spun ribbons.
  • This ranking order does not simply follow the order of magnitude of the Cr V content in the amorphous alloys, but is particular to the elemental form.
  • the highest electrocatalytic activity of Ni 50 Co 25 V 5 B 20 amongst the amo ⁇ hous alloys could possibly be attributed to the synergetic effect of Ni-Co-V that may influence the nature of the oxide film formed on this amo ⁇ hous alloy.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Electrochemistry (AREA)
  • Ceramic Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

La présente invention concerne des électrodes en verre métallique/métal amorphe produites par solidification rapide, (a) présentant une structure qui est soit amorphe soit nanocristalline, (b) contenant le principal élément d'alliage Ni, (c) contenant des additions d'alliage de Co et au moins un élément du groupe IVB, VB, VIB, VIIB et/ou VIIIB, de préférence Cr et V, dans des proportions comprises entre 0 et 20 atomes pour cent, et lorsqu'elles sont associées au Ni, elles représentent entre 0,75 et 0,85 de la fraction atomique de l'alliage, et (d) contenant des éléments métalloïdes comprenant de préférence un ou plusieurs éléments C, B, Si et P, individuellement ou associés, pour représenter entre 0,15 et 0,25 fraction atomique de l'alliage. Ces électrodes présentent une excellente stabilité thermique, une stabilité améliorée dans un électrolyte aqueux et peuvent fournir une efficacité de courant améliorée (rendement de surtension anodique). Ces électrodes sont utilisées dans l'électrolyse de solutions d'électrolytes aqueux, comme par exemple les mélanges de caustique et d'eau, dans la production d'oxygène et d'hydrogène.
PCT/CA2000/001251 1999-10-26 2000-10-23 Electrodes en metal amorphe/verre metallique pour procedes electrochimiques WO2001031085A2 (fr)

Priority Applications (7)

Application Number Priority Date Filing Date Title
JP2001533216A JP2003513170A (ja) 1999-10-26 2000-10-23 電気化学方法用の非晶質金属／金属ガラス電極
BR0014994-2A BR0014994A (pt) 1999-10-26 2000-10-23 Vidro metálico para uso em processos eletroquìmicos, eletrodo para uso em uma célula eletroquìmica, e, processo para a produção eletroquìmica de oxigênio e hidrogênio a partir de uma solução aquosa em uma célula eletroquìmica
EP00971182A EP1230412A2 (fr) 1999-10-26 2000-10-23 Electrodes en metal amorphe/verre metallique pour procedes electrochimiques
MXPA02002673A MXPA02002673A (es) 1999-10-26 2000-10-23 Electrodos de metal amorfo/vidrio metalico para procesos electroquimicos.
KR1020027004542A KR20020037772A (ko) 1999-10-26 2000-10-23 전기화학 공정용 비정질금속/금속유리 전극
AU10135/01A AU1013501A (en) 1999-10-26 2000-10-23 Amorphous metal/metallic glass electrodes for electrochemical processes
NO20020957A NO20020957L (no) 1999-10-26 2002-02-27 Amorfe metall/metallklaff-elektroder for elektrokjemiske prosesser

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CA002287648A CA2287648C (fr) 1999-10-26 1999-10-26 Electrodes de metal amorphe/verre metallique pour processus electrochimiques
CA2,287,648 1999-10-26

Publications (2)

Publication Number Publication Date
WO2001031085A2 true WO2001031085A2 (fr) 2001-05-03
WO2001031085A3 WO2001031085A3 (fr) 2001-09-20

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Country Status (11)

Country Link
EP (1) EP1230412A2 (fr)
JP (1) JP2003513170A (fr)
KR (1) KR20020037772A (fr)
CN (1) CN1382229A (fr)
AU (1) AU1013501A (fr)
BR (1) BR0014994A (fr)
CA (1) CA2287648C (fr)
MX (1) MXPA02002673A (fr)
NO (1) NO20020957L (fr)
WO (1) WO2001031085A2 (fr)
ZA (1) ZA200201857B (fr)

Cited By (19)

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Publication number Priority date Publication date Assignee Title
WO2012010941A1 (fr) * 2010-07-21 2012-01-26 Rolex S.A. Composant horloger comprenant un alliage métallique amorphe
US8668847B2 (en) 2010-08-13 2014-03-11 Samsung Electronics Co., Ltd. Conductive paste and electronic device and solar cell including an electrode formed using the conductive paste
US8715535B2 (en) 2010-08-05 2014-05-06 Samsung Electronics Co., Ltd. Conductive paste and electronic device and solar cell including an electrode formed using the conductive paste
US8764963B2 (en) 2007-11-16 2014-07-01 Akzo Nobel N.V. Electrode
US8940195B2 (en) 2011-01-13 2015-01-27 Samsung Electronics Co., Ltd. Conductive paste, and electronic device and solar cell including an electrode formed using the same
US8974703B2 (en) 2010-10-27 2015-03-10 Samsung Electronics Co., Ltd. Conductive paste and electronic device and solar cell including an electrode formed using the same
US8987586B2 (en) 2010-08-13 2015-03-24 Samsung Electronics Co., Ltd. Conductive paste and electronic device and solar cell including an electrode formed using the conductive paste
US9039940B2 (en) 2011-03-25 2015-05-26 Samsung Electronics Co., Ltd. Conductive paste and electronic device, and solar cell including an electrode formed using the conductive paste
US9039943B2 (en) 2011-03-28 2015-05-26 Samsung Electronics Co., Ltd. Conductive paste and electronic device and solar cell including an electrode formed using the conductive paste
US9105370B2 (en) 2011-01-12 2015-08-11 Samsung Electronics Co., Ltd. Conductive paste, and electronic device and solar cell including an electrode formed using the same
US9218898B2 (en) 2011-12-09 2015-12-22 Samsung Electronics Co., Ltd. Conductive paste and electronic device and solar cell including an electrode formed using the conductive paste
US9228625B2 (en) 2010-07-21 2016-01-05 Rolex S.A. Amorphous metal alloy
US9433928B2 (en) 2011-09-01 2016-09-06 Click Materials Corp. Electrocatalytic materials and methods for manufacturing same
US9947809B2 (en) 2009-11-11 2018-04-17 Samsung Electronics Co., Ltd. Conductive paste and electronic device and solar cell including an electrode formed using the conductive paste
US9984787B2 (en) 2009-11-11 2018-05-29 Samsung Electronics Co., Ltd. Conductive paste and solar cell
US10399166B2 (en) 2015-10-30 2019-09-03 General Electric Company System and method for machining workpiece of lattice structure and article machined therefrom
KR20190111863A (ko) * 2019-09-23 2019-10-02 삼성전자주식회사 투명 도전체 및 그 제조 방법과 상기 투명 도전체를 포함하는 전자 소자
CN114192749A (zh) * 2020-09-17 2022-03-18 南京理工大学 基于腐蚀非晶合金阳极材料进行电沉积制备纳米材料的方法
CN114672716A (zh) * 2022-04-11 2022-06-28 大连理工大学 一种热处理态下高强韧性的CoCrNi2(V2B)x共晶高熵合金及其制备方法

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KR100647672B1 (ko) 2004-12-24 2006-11-23 삼성에스디아이 주식회사 내열성 투명 전극, 이의 제조방법 및 이를 구비한염료감응 태양 전지
JP4992085B2 (ja) * 2007-02-23 2012-08-08 国立大学法人東京工業大学 無電解めっき用膜状触媒組成物
KR101741682B1 (ko) 2010-08-24 2017-05-31 삼성전자주식회사 도전성 페이스트와 상기 도전성 페이스트를 사용하여 형성된 전극을 포함하는 전자 소자 및 태양 전지
JP5822235B2 (ja) * 2012-06-08 2015-11-24 住友金属鉱山エンジニアリング株式会社 酸化態窒素の除去方法
KR101999795B1 (ko) 2012-06-27 2019-07-12 삼성전자주식회사 도전성 페이스트, 상기 도전성 페이스트를 사용하여 형성된 전극을 포함하는 전자 소자 및 태양 전지
EP2978868A4 (fr) * 2013-07-12 2017-01-04 Hewlett-Packard Development Company L.P. Film métallique mince amorphe
JP5949792B2 (ja) * 2014-01-15 2016-07-13 株式会社豊田中央研究所 結晶質電極材および不溶性電極
US10177310B2 (en) 2014-07-30 2019-01-08 Hewlett Packard Enterprise Development Lp Amorphous metal alloy electrodes in non-volatile device applications
CN108660474B (zh) * 2018-06-01 2020-02-07 北京航空航天大学 (FeaCobNic)xMyRz系析氧催化材料及在阳极析氧电极上的应用
CN115558951A (zh) * 2022-10-18 2023-01-03 海南大学 非晶纳米多孔镍合金一体式电极、制备方法及其应用

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US8764963B2 (en) 2007-11-16 2014-07-01 Akzo Nobel N.V. Electrode
US9984787B2 (en) 2009-11-11 2018-05-29 Samsung Electronics Co., Ltd. Conductive paste and solar cell
US9947809B2 (en) 2009-11-11 2018-04-17 Samsung Electronics Co., Ltd. Conductive paste and electronic device and solar cell including an electrode formed using the conductive paste
US9228625B2 (en) 2010-07-21 2016-01-05 Rolex S.A. Amorphous metal alloy
WO2012010941A1 (fr) * 2010-07-21 2012-01-26 Rolex S.A. Composant horloger comprenant un alliage métallique amorphe
US9315884B2 (en) 2010-07-21 2016-04-19 Rolex Sa Watch-making or clock-making component comprising an amorphous metal alloy
US8715535B2 (en) 2010-08-05 2014-05-06 Samsung Electronics Co., Ltd. Conductive paste and electronic device and solar cell including an electrode formed using the conductive paste
US8668847B2 (en) 2010-08-13 2014-03-11 Samsung Electronics Co., Ltd. Conductive paste and electronic device and solar cell including an electrode formed using the conductive paste
US8987586B2 (en) 2010-08-13 2015-03-24 Samsung Electronics Co., Ltd. Conductive paste and electronic device and solar cell including an electrode formed using the conductive paste
US8974703B2 (en) 2010-10-27 2015-03-10 Samsung Electronics Co., Ltd. Conductive paste and electronic device and solar cell including an electrode formed using the same
US9105370B2 (en) 2011-01-12 2015-08-11 Samsung Electronics Co., Ltd. Conductive paste, and electronic device and solar cell including an electrode formed using the same
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WO2001031085A3 (fr) 2001-09-20
CA2287648C (fr) 2007-06-19
EP1230412A2 (fr) 2002-08-14
NO20020957D0 (no) 2002-02-27
BR0014994A (pt) 2002-06-18
JP2003513170A (ja) 2003-04-08
AU1013501A (en) 2001-05-08
ZA200201857B (en) 2002-12-24
KR20020037772A (ko) 2002-05-22
MXPA02002673A (es) 2003-10-14
CA2287648A1 (fr) 2001-04-26
CN1382229A (zh) 2002-11-27

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