WO2017081587A1 - Electrocatalyst for the reduction of oxygen - Google Patents

Electrocatalyst for the reduction of oxygen Download PDF

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Publication number
WO2017081587A1
WO2017081587A1 PCT/IB2016/056642 IB2016056642W WO2017081587A1 WO 2017081587 A1 WO2017081587 A1 WO 2017081587A1 IB 2016056642 W IB2016056642 W IB 2016056642W WO 2017081587 A1 WO2017081587 A1 WO 2017081587A1
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WO
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Prior art keywords
electrocatalyst
metals
value
platinum
orr
Prior art date
Application number
PCT/IB2016/056642
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French (fr)
Inventor
Roelof Jacobus KRIEK
Anzel FALCH
Original Assignee
North-West University
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 North-West University filed Critical North-West University
Publication of WO2017081587A1 publication Critical patent/WO2017081587A1/en
Priority to ZA2018/02926A priority Critical patent/ZA201802926B/en

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Classifications

    • 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
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/02—Hydrogen or oxygen
    • C25B1/04—Hydrogen or oxygen by electrolysis of water
    • 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
    • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
    • 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
    • H01M4/90—Selection of catalytic material
    • H01M4/9041—Metals or alloys
    • 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
    • H01M4/90—Selection of catalytic material
    • H01M4/92—Metals of platinum group
    • H01M4/921—Alloys or mixtures with metallic elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
    • B01J23/892—Nickel and noble metals
    • 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
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
    • 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 present invention relates to an electrocatalyst for use in the reduction of oxygen.
  • the invention further extends to an electrolytic reactor provided with said electrocatalyst and a method for the reduction of water using the aforementioned electrolytic reactor.
  • ORR oxygen reduction reaction
  • the ORR takes place in acidic and alkaline medium.
  • the reactions for the different media are listed below.
  • Acidic aqueous solutions 0 2 + H* + 1 ⁇ 2r ⁇ H 2 0 3 ⁇ 4£3 ⁇ 4 + 2M * + 2e - ⁇ 23 ⁇ 4
  • An electrocatalyst is a catalyst that participates in electrochemical reactions. Catalyst materials modify and increase the rate of chemical reactions without being consumed in the process. Electrocatalysts provide a specific form of catalysts that function at electrode surfaces or may be the electrode surface itself.
  • An electrocatalyst can be heterogeneous such as a platinum surface or nanoparticles, or homogeneous like a coordination complex or enzyme.
  • the electrocatalyst typically assists in transferring electrons between the electrode and reactants, and/or facilitates an intermediate chemical transformation described by an overall half-reaction.
  • US patent application 2014205928 describes an alloy catalyst PtXY, wherein X is nickel, cobalt, chromium, copper, titanium or manganese and Y is tantalum or niobium, characterised in that in the alloy the atomic percentage of platinum is 46-75 at %, of X is 1 -49 at % and of Y is 1 -35 at %; provided that the alloy is not 66 at % Pt 20 at % CM 4 at % Ta or 50 at % Pt, 25 at % Co, 25 at % Ta.
  • the alloy is held as being particularly suitable for use as a catalyst in oxygen reduction.
  • US patent 8,895,206 describes a poms metal comprising platinum; wherein said porous metal has a specific surface area that is greater than 5 m 2 /g and less than 75 m 2 /g; for use in oxygen reduction.
  • a common disadvantage of known electrocatalysts is that they have a relatively inefficient onset energy level and current density, with pure platinum electrocatalysts for oxygen reduction providing a benchmark level and density, which has hardly ever been improved on in the past.
  • an electrocatalyst for use in the oxygen reduction reaction including a combination of two or more metals described by the following formula:
  • R is one or more metals selected from the platinum-group metals; x has a value of from 1 to 40;
  • y has a value of from 25 to 70;
  • z has a value of from 1 to 20.
  • an electrocatalyst for use in the oxygen reduction reaction ORR
  • the electrocatalsyt being provided as a combination of two or more metals described by the following formula:
  • R is one or more metals selected from the platinum-group metals; x has a value of from 1 to 30;
  • y has a value of from 25 to 70;
  • the platinum group metals are selected from the group consisting of platinum, iridium, and combinations thereof.
  • the combination of metals forming the electrocatalyst may be deposited on an electrode (cathode and/or anode) by means of the sputtering technique, as known in the art.
  • the combination of metals forming the electrocatalyst may be deposited on an electrode by means of nanoparticle deposition, as known in the art.
  • electrocatalyst a number of other known techniques for the production of an electrocatalyst may be used, such as electrochemical deposition, hot dipping or alloying of the electrocatalytic metals.
  • R is platinum with x having a value of from 20 to 40, y of from 50 to 70 and z of from 5 to 15.
  • a reactor for use in the ORR the reactor being provided with an electrocatalyst according to the first aspect of the invention.
  • the ORR will be readily understood by persons knowledgeable in the art as including both the alkaline and acidic forms of the reaction.
  • the reaction is the alkaline ORR.
  • Figure 1 is a representation of linear sweep voltammetry for a number of platinum-containing electrocatalysts.
  • the electrocatalyst according to a preferred embodiment of the invention is particularly suitable for use in the Oxygen Reduction Reaction (ORR) using a reactor (not shown) having an anode and a cathode located in a container for an electrolyte.
  • the electrolyte is typically an alkaline solution such as potassium chloride.
  • the electrocatalyst is provided as a combination of metals described by the following formula: R Ni y Al z wherein:
  • R is one or more metals selected from the platinum-group metals; x has a value of from 1 to 40;
  • y has a value of from 25 to 70;
  • z has a value of from 1 to 20.
  • the platinum group metals are selected from the group consisting of platinum, iridium and combinations thereof. More preferably, R is platinum with x having a value of from 20 to 40, y of from 50 to 70 and z of from 5 to 15.
  • a deposition head is used to coat the electrode/s with a preselected metal or mixture of metals (electrocatalysts) according to the invention, to be screened and tested in a manner known in the art and substantially as described in US patent 6,756,109.
  • the electrocatalyst is deposited on the electrode/s by means of a sputtering technique, as known in the art. In this instance evaporative sputtering is used, with a combinatorial approach being adopted for rapid development and screening of electrocatalyst compositions.
  • sputtering is proceeded by calibration of the device in order to reduce deposition rate/power curves for all electrocatalysts being deposited. Sputtering is carried out under a low-pressure argon atmosphere. Following calibration, deposition is carried out individually for each electrode in an array.
  • the array is then placed in the container, which is filled with an appropriate electrolytic solution. Contacts are connected to a 64-channel potentiostat (not shown). Electrochemical reactions are carried out within the container, with the results being recorded for each electrode in an array. This allows for a number of different electrocatalysts deposited on the electrodes to be screened and tested during the same reaction, allowing combinatorial screening of a number of different electrode constituents and coatings (forming the electrocatalysts) at the same time. The known potential difference across electrodes allows measurement of the relative current densities of different electrocatalysts in comparison to a counter electrode.

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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)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)

Abstract

The present invention relates to an electrocatalyst for use in the reduction of oxygen. The invention further extends to a reactor provided with said electrocatalyst and a method for the oxygen reduction reaction (ORR) using the aforementioned reactor. According to a first (and second) aspect of the invention, there is provided an electrocatalyst for use in the ORR, the electrocatalyst being provided as a combination of three or more metals described by the following formula: RxNiyAlz,wherein: R is one or more metals selected from the platinum-group metals; x has a value of from 1 to 40 (1 to 30); y has a value of from 25 to 70 (25 to 70); and z has a value of from 1 to 20 (25 to 70).

Description

ELECTROCATALYST FOR THE REDUCTION OF OXYGEN
FIELD OF THE INVENTION The present invention relates to an electrocatalyst for use in the reduction of oxygen. The invention further extends to an electrolytic reactor provided with said electrocatalyst and a method for the reduction of water using the aforementioned electrolytic reactor. BACKGROUND TO THE INVENTION
The oxygen reduction reaction (ORR) finds application in fuel cells, which are widely researched and developed for power generation; in new generation motor vehicles; and in backup power modules.
The ORR takes place in acidic and alkaline medium. The reactions for the different media are listed below.
Acidic aqueous solutions: 02 + H* + ½r→ H20 ¾£¾ + 2M * + 2e -→ 2¾
Alkaline aqueous solutions:
02 + H20 + 4 ~→WH~ 02 + H20 + 2e -→ HQz + QH-
HQ~ + H20 + 2e~→ 3ϋΗ~
An electrocatalyst is a catalyst that participates in electrochemical reactions. Catalyst materials modify and increase the rate of chemical reactions without being consumed in the process. Electrocatalysts provide a specific form of catalysts that function at electrode surfaces or may be the electrode surface itself.
An electrocatalyst can be heterogeneous such as a platinum surface or nanoparticles, or homogeneous like a coordination complex or enzyme. The electrocatalyst typically assists in transferring electrons between the electrode and reactants, and/or facilitates an intermediate chemical transformation described by an overall half-reaction.
Various electrocatalysts are known and used in the reduction of oxygen. For example, US patent application 2014205928 describes an alloy catalyst PtXY, wherein X is nickel, cobalt, chromium, copper, titanium or manganese and Y is tantalum or niobium, characterised in that in the alloy the atomic percentage of platinum is 46-75 at %, of X is 1 -49 at % and of Y is 1 -35 at %; provided that the alloy is not 66 at % Pt 20 at % CM 4 at % Ta or 50 at % Pt, 25 at % Co, 25 at % Ta. The alloy is held as being particularly suitable for use as a catalyst in oxygen reduction.
In a further example US patent 8,895,206 describes a poms metal comprising platinum; wherein said porous metal has a specific surface area that is greater than 5 m2/g and less than 75 m2/g; for use in oxygen reduction.
A common disadvantage of known electrocatalysts is that they have a relatively inefficient onset energy level and current density, with pure platinum electrocatalysts for oxygen reduction providing a benchmark level and density, which has hardly ever been improved on in the past.
OBJECT OF THE INVENTION
There is thus a need in the art for an electrocatalyst that performs relatively better than a pure platinum electrocatalyst in the reduction of oxygen and it is an object of the present invention to provide such an electrocatalyst. SUMMARY OF THE INVENTION
According to a first aspect of the invention, there is provided an electrocatalyst for use in the oxygen reduction reaction (ORR), the electrocatalyst including a combination of two or more metals described by the following formula:
R NiyAlz wherein:
R is one or more metals selected from the platinum-group metals; x has a value of from 1 to 40;
y has a value of from 25 to 70; and
z has a value of from 1 to 20.
According to a second aspect of the invention, there is provided an electrocatalyst for use in the oxygen reduction reaction (ORR), the electrocatalsyt being provided as a combination of two or more metals described by the following formula:
R NiyAlz wherein:
R is one or more metals selected from the platinum-group metals; x has a value of from 1 to 30;
y has a value of from 25 to 70; and
z has a value of from 25 to 70. Preferably, the platinum group metals are selected from the group consisting of platinum, iridium, and combinations thereof.
In an embodiment of the invention, the combination of metals forming the electrocatalyst may be deposited on an electrode (cathode and/or anode) by means of the sputtering technique, as known in the art. Alternatively, the combination of metals forming the electrocatalyst may be deposited on an electrode by means of nanoparticle deposition, as known in the art.
It may further readily be appreciated that a number of other known techniques for the production of an electrocatalyst may be used, such as electrochemical deposition, hot dipping or alloying of the electrocatalytic metals.
According to a preferred embodiment of the invention; R is platinum with x having a value of from 20 to 40, y of from 50 to 70 and z of from 5 to 15.
According to a third aspect of the invention, there is provided a reactor for use in the ORR, the reactor being provided with an electrocatalyst according to the first aspect of the invention. The ORR will be readily understood by persons knowledgeable in the art as including both the alkaline and acidic forms of the reaction. In a preferred embodiment, the reaction is the alkaline ORR.
According to a fourth aspect of the invention, there is provided a method for the ORR using a reactor according to the second embodiment of the invention.
According to a fifth aspect of the invention, there is provided for the use of the reactor according to the second embodiment of the invention in the electrolysis of water.
BRIEF DESCRIPTION OF THE FIGURES The invention will now be described further, by way of example only, with reference to accompanying figures wherein:
Figure 1 is a representation of linear sweep voltammetry for a number of platinum-containing electrocatalysts.
DETAILED DESCRIPTION OF THE INVENTION
An electrocatalyst according to a preferred embodiment of the invention will now be described by way of example only. The electrocatalyst according to the invention is particularly suitable for use in the Oxygen Reduction Reaction (ORR) using a reactor (not shown) having an anode and a cathode located in a container for an electrolyte. The electrolyte is typically an alkaline solution such as potassium chloride.
The electrocatalyst is provided as a combination of metals described by the following formula: R NiyAlz wherein:
R is one or more metals selected from the platinum-group metals; x has a value of from 1 to 40;
y has a value of from 25 to 70; and
z has a value of from 1 to 20.
Preferably, the platinum group metals are selected from the group consisting of platinum, iridium and combinations thereof. More preferably, R is platinum with x having a value of from 20 to 40, y of from 50 to 70 and z of from 5 to 15.
A deposition head is used to coat the electrode/s with a preselected metal or mixture of metals (electrocatalysts) according to the invention, to be screened and tested in a manner known in the art and substantially as described in US patent 6,756,109. Preferably the electrocatalyst is deposited on the electrode/s by means of a sputtering technique, as known in the art. In this instance evaporative sputtering is used, with a combinatorial approach being adopted for rapid development and screening of electrocatalyst compositions.
In use, sputtering is proceeded by calibration of the device in order to reduce deposition rate/power curves for all electrocatalysts being deposited. Sputtering is carried out under a low-pressure argon atmosphere. Following calibration, deposition is carried out individually for each electrode in an array.
The array is then placed in the container, which is filled with an appropriate electrolytic solution. Contacts are connected to a 64-channel potentiostat (not shown). Electrochemical reactions are carried out within the container, with the results being recorded for each electrode in an array. This allows for a number of different electrocatalysts deposited on the electrodes to be screened and tested during the same reaction, allowing combinatorial screening of a number of different electrode constituents and coatings (forming the electrocatalysts) at the same time. The known potential difference across electrodes allows measurement of the relative current densities of different electrocatalysts in comparison to a counter electrode. In comparing various combinations of electrocatalysts in accordance with the formula according to the invention, optimal combinations of electrocatalytic metals were identified (as shown in Figure 1 ). A well-accepted measure of catalytic efficiency for this process lies in comparing the onset potential and current density obtained when testing a putative catalyst against both the existing state of the art and maximum values expected under ideal conditions. During operation, it was surprisingly found that the onset potential of the electrode was significantly lower when compared to existing platinum and platinum-alloy catalysts used currently in the art. Similarly, the current density of the catalyst material was surprisingly found to be raised when compared to existing platinum and platinum-alloy catalysts at the same level of potential.
It will be appreciated that variations in detail are possible with an electrocatalyst according to the invention, without departing from the scope and/or spirit of this disclosure.

Claims

1 . An electrocatalyst for use in the Oxygen Reduction Reaction (ORR), the electrocatalyst including a combination of two or more metals described by the following formula:
R NiyAlz wherein:
R is one or more metals selected from the platinum-group metals; x has a value of from 1 to 40;
y has a value of from 25 to 70; and
z has a value of from 1 to 20.
2. An electrocatalyst for use in the Oxygen Reduction Reaction (ORR), the electrocatalyst including a combination of two or more metals described by the following formula:
R NiyAlz wherein:
R is one or more metals selected from the platinum-group metals; x has a value of from 1 to 30;
y has a value of from 25 to 70; and z has a value of from 25 to 70.
The electrocatalyst of claim 1 ; wherein R is platinum with x having a value of from 20 to 40, y of from 50 to 70 and z of from 5 to 15.
The electrocatalyst of either claim 1 or claim 2, wherein the platinum group metals are selected from the group consisting of platinum, iridium and combinations thereof.
The electrocatalyst of any of claims 1 to 4, wherein the combination of metals forming the electrocatalyst is deposited on an electrode by means of the sputtering technique.
The electrocatalyst of any of claims 1 to 5, wherein the combination of metals forming the electrocatalyst is deposited on an electrode by means of nanoparticle deposition.
An electrolytic reactor for use in the ORR using the electrocatalyst of any of claims 1 to 6.
A method for the ORR using the electrolytic reactor of claim 7.
9. The use of the electrolytic reactor of claim 7 in the ORR.
10. The electrocatalyst of either claim 1 or claim 2, substantially as herein described and/or exemplified with reference to the accompanying figures.
1 1 . The electrolytic reactor of claim 7, substantially as herein described and/or exemplified with reference to the accompanying figures.
12. The method of claim 8, substantially as herein described and/or exemplified with reference to the accompanying figures.
13. The use of claim 9, substantially as herein described and/or exemplified with reference to the accompanying figures.
PCT/IB2016/056642 2015-11-13 2016-11-04 Electrocatalyst for the reduction of oxygen WO2017081587A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
ZA2018/02926A ZA201802926B (en) 2015-11-13 2018-05-04 Electrocatalyst for the reduction of oxygen

Applications Claiming Priority (4)

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ZA201508425 2015-11-13
ZA2015/08425 2015-11-13
ZA201606585 2016-09-23
ZA2016/06585 2016-09-23

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5925985A (en) * 1982-08-03 1984-02-10 Asahi Glass Co Ltd Low overvoltage cathode having high durability and its production
US4498962A (en) * 1982-07-10 1985-02-12 Agency Of Industrial Science And Technology Anode for the electrolysis of water
US4746584A (en) * 1985-06-24 1988-05-24 The Standard Oil Company Novel amorphous metal alloys as electrodes for hydrogen formation and oxidation
US6756109B2 (en) 1997-09-30 2004-06-29 Symyx Technologies, Inc. Combinatorial electrochemical deposition and testing system
US20110177432A1 (en) * 2009-05-28 2011-07-21 The Johns Hopkins University Porous metal catalysts for oxygen reduction
US20140205928A1 (en) 2009-02-11 2014-07-24 Johnson Matthey Fuel Cells Limited Ternary platinum alloy catalyst

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4498962A (en) * 1982-07-10 1985-02-12 Agency Of Industrial Science And Technology Anode for the electrolysis of water
JPS5925985A (en) * 1982-08-03 1984-02-10 Asahi Glass Co Ltd Low overvoltage cathode having high durability and its production
US4746584A (en) * 1985-06-24 1988-05-24 The Standard Oil Company Novel amorphous metal alloys as electrodes for hydrogen formation and oxidation
US6756109B2 (en) 1997-09-30 2004-06-29 Symyx Technologies, Inc. Combinatorial electrochemical deposition and testing system
US20140205928A1 (en) 2009-02-11 2014-07-24 Johnson Matthey Fuel Cells Limited Ternary platinum alloy catalyst
US20110177432A1 (en) * 2009-05-28 2011-07-21 The Johns Hopkins University Porous metal catalysts for oxygen reduction
US8895206B2 (en) 2009-05-28 2014-11-25 The Johns Hopkins University Porous platinum-based catalysts for oxygen reduction

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