US20150114834A1 - Surface modified electrodes for electrochemical syngas production - Google Patents

Surface modified electrodes for electrochemical syngas production Download PDF

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Publication number
US20150114834A1
US20150114834A1 US14/068,291 US201314068291A US2015114834A1 US 20150114834 A1 US20150114834 A1 US 20150114834A1 US 201314068291 A US201314068291 A US 201314068291A US 2015114834 A1 US2015114834 A1 US 2015114834A1
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Prior art keywords
electrode
metal substrate
carbon monoxide
self
organic functional
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US14/068,291
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English (en)
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Hongfei Jia
Kenneth James McDonald
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Toyota Motor Engineering and Manufacturing North America Inc
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Toyota Motor Engineering and Manufacturing North America Inc
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Priority to US14/068,291 priority Critical patent/US20150114834A1/en
Assigned to TOYOTA MOTOR ENGINEERING & MANUFACTURING NORTH AMERICA, INC. reassignment TOYOTA MOTOR ENGINEERING & MANUFACTURING NORTH AMERICA, INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: JIA, HONGFEI, MCDONALD, KENNETH JAMES
Priority to DE201410114658 priority patent/DE102014114658A1/de
Priority to CN201410539635.9A priority patent/CN104593817B/zh
Priority to JP2014218106A priority patent/JP6485857B2/ja
Publication of US20150114834A1 publication Critical patent/US20150114834A1/en
Priority to US16/667,292 priority patent/US20200063275A1/en
Abandoned legal-status Critical Current

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    • 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
    • C25B11/0405—
    • 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
    • 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
    • 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
    • C25B1/23—Carbon monoxide or syngas
    • 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
    • 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
    • C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
    • 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
    • C25B11/097—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 comprising two or more noble metals or noble metal alloys
    • 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

Definitions

  • the invention relates to electrodes for carbon dioxide reduction and with more particularity to electrodes having a self-assembled monolayer applied thereon for carbon dioxide reduction.
  • Fossil fuels are a finite resource that is utilized for various functions such as a fuel source or feed stock for various products.
  • the burning of fossil fuels increases the amount of CO 2 in the environment.
  • Electrolysis cells may be utilized for electrochemical reduction of CO 2 in aqueous medium to produce a variety of products such as H 2 , CO, alcohols, formic acid, methane and short-chain alkanes.
  • H 2 , CO, alcohols, formic acid, methane and short-chain alkanes are highly desired because it can serve as feedstock to commercial Fischer-Tropsch processes for the production of liquid hydrocarbons. Selectively producing H 2 and CO at a controlled ratio would benefit the Fisher-Tropsch process.
  • an electrode for electrochemical reduction of carbon dioxide and water forming carbon monoxide and hydrogen includes a metal substrate.
  • a self-assembled monolayer is bonded to the metal substrate.
  • a selectivity of reaction products of carbon monoxide and hydrogen produced by the electrode is regulated relative to a bare metal substrate.
  • an electrode for electrochemical reduction of carbon dioxide and water forming carbon monoxide and hydrogen includes a metal substrate.
  • a self-assembled monolayer is bonded to the metal substrate.
  • the self-assembled monolayer includes an organic ligand having a surface end having a reactive group bonded to the metal substrate and an opposing end including an organic functional group.
  • a selectivity of reaction products of carbon monoxide and hydrogen produced by the electrode is regulated relative to a bare metal substrate.
  • an electrode for electrochemical reduction of carbon dioxide and water forming carbon monoxide and hydrogen includes a metal substrate.
  • a self-assembled monolayer is bonded to the metal substrate.
  • An activity of the electrode is regulated relative to a bare metal substrate.
  • FIG. 1 is a schematic representation of a self-assembled monolayer attached to a metal substrate
  • FIG. 2 is a CV plot of a gold metal substrate having a self-assembling monolayer having ligands attached with the ligands including various organic functional groups and a measurement of the water contact angle for the ligands including various organic functional groups;
  • FIG. 3 is a CV plot of a silver metal substrate having a self-assembling monolayer having ligands attached with the ligands including various organic functional groups;
  • FIG. 4 is a plot of the potentiostatic polarization of silver substrates having a self-assembling monolayer having ligands attached with the ligands including various organic functional groups;
  • FIG. 5 is gas chromatography plots of silver substrates having a self-assembling monolayer having ligands attached with the ligands including various organic functional groups and a percentage of hydrogen and carbon monoxide in a gas phase product;
  • FIG. 6 are plots of the ratio of carbon monoxide to hydrogen for silver and gold substrates having a self-assembling monolayer having C2 and C11 length ligands attached with the ligands including various organic functional groups;
  • FIG. 7 are plots of the activity for gold substrates having a self-assembling monolayer having C2 and C11 length ligands attached with the ligands including various organic functional groups;
  • FIG. 8 is a pictorial diagram of an experimental electrochemical cell including a wire working electrode.
  • FIG. 1 there is shown a diagram of an electrode 10 for electrochemical reduction of carbon dioxide and water forming carbon monoxide and hydrogen.
  • the electrode includes a metal substrate 15 .
  • a self-assembled monolayer 20 is bonded to the metal substrate 15 .
  • the reaction products of the electrochemical reduction of carbon dioxide and water may produce a syngas formed of carbon monoxide and hydrogen.
  • the syngas may be utilized in a Fischer-Tropsch Process as detailed by the reaction below to produce various hydrocarbon materials.
  • the efficiency and productivity for a desired hydrocarbon from the Fischer-Tropsch Process can be increased. For example, it may be desirable to have a ratio of 2:1 of hydrogen to carbon monoxide for the synthesis of a liquid hydrocarbon fuel, such as gasoline.
  • the metal substrate 15 may be formed of a metal having a low carbon monoxide bonding strength.
  • the bond strength may be characterized such that the CO adsorption energy is less than 1 eV.
  • the metals may be selected from Au, Ag, Zn, Pd, and Ga.
  • the self-assembled monolayer 20 includes an organic ligand 25 having a surface end 30 having a reactive group 35 bonded to the metal substrate 15 and an opposing end 40 including an organic functional group 45 .
  • the organic ligand may have a length of carbon units of from C2 to C20.
  • the ligand may be formed of alkane chains or aromatic chains.
  • the reactive group forms a covalent bond with the metal substrate.
  • the reactive group may include a thiol group.
  • the thiol groups of the reactive group may react with the surface of the metal substrate to form a covalent bond.
  • the ligands are assembled on the metal substrate as a monolayer as depicted in FIG. 1 .
  • the opposing end may include an organic functional group that may be selected from CH 3 , OH, COOH and NH 2 .
  • the organic functional group may be exposed to an aqueous electrolyte that is saturated with carbon dioxide.
  • the various organic functional groups may affect various properties of the electrode including the hydrophobicity as well as the charge at the electrolyte interface. The changes in electrode properties may be utilized to regulate or modify the selectivity and activity of the electrode.
  • Gold (Au) and Silver (Ag) thin film electrodes (100 nm in thickness) were prepared by LGA Thin Film Inc. (Santa Clara, Calif.) using sputtering. To increase adhesion, a 20-nm layer of Ti was pre-sputtered on glass substrate prior to the deposition of Au or Ag films.
  • Ag wire electrodes (1.0 mm in diameter), Thio-based ligands, potassium bicarbonate (KHCO 3 ) and ethanol were purchased from Sigma Aldrich.
  • Assembly of ligands on metal substrate of the electrode includes substrate cleaning, preparation of ligand solution, incubation for assembly and post-assembly rinsing.
  • the electrodes were sonicated first in DI water (5 min, twice) and then in ethanol (5 min, twice).
  • the surface was mechanically polished with 50 nm Al2O3 prior to the cleaning procedures.
  • Electrochemical analysis was conducted in a two chamber cell as shown in FIG. 8 , using Pt mesh as counter and Ag/AgCl as reference electrodes, respectively.
  • KHCO 3 (0.1 M) was used as an electrolyte. CO 2 was purged through the electrolyte for at least 15 min before starting the experiment.
  • cyclic voltammetry studies and water contact angle measurements were performed on thin film electrodes for Au and Ag metal substrates.
  • Ag wire electrodes were utilized for potentiostatic electrolysis and GC analysis.
  • the anode and cathode chambers were separated by a piece of Nafion 117.
  • 25 ml of electrolyte was filled into the anode chamber, which allowed 5.5 ml of gas phase volume in the headspace.
  • SAM self-assembled monolayers
  • C-2 and C-11 ligands were also applied to the modification of Ag wire electrodes, which were then used for bulk electrolysis.
  • potentiostatic electrolysis was conducted at potentials ranging from ⁇ 0.8 to ⁇ 1.6 V (vs. Ag/AgCl). Because the SAM ligands have non-conductive alkane chains, it can be expected that the modified electrodes would be less active than the blank control, as shown in FIG. 4 . This result confirms ligand attachment to Ag surface.
  • the SAM modified electrodes were less active than the blank Ag control, indicating the ligands might have created insulating barriers for electron transfer to affect the activity of the electrodes such that the activity may be regulated or controlled.
  • the amount of H 2 and CO product in the electrochemical cell headspace was measured by gas chromatography (GC) after a total pass of one coulomb of charge.
  • GC gas chromatography
  • SAM-modification has significant influences on catalyst selectivity.
  • the calculated ratios are summarized in the table of FIG. 5 for a C-11 ligand having various organic functional groups.
  • the ratio of H 2 to CO increases from —COOH to —CH 2 OH and —CH 3 , correlating well with surface hydrophobility.
  • the —NH 2 functional group showed the highest ratio of H 2 to CO.
  • FIG. 6 there is shown a plot detailing the ratio of carbon monoxide to hydrogen for silver and gold metal substrates having SAM applied to the surfaces of the electrode and including various functional groups.
  • the plots include both C-2 and C-11 length ligands.
  • the plots were generated utilizing the experimental apparatus described above with CO2 saturated 0.1M KHCO3 as an electrolyte at a pH of 6.8 at a constant potential of ⁇ 1.5 V (vs. Ag/AgCl).
  • the ligand length, metal substrate and the choice of organic functional group may be selected to regulate the selectivity of the electrode reaction products of carbon monoxide and hydrogen produced by the electrode.
  • FIG. 7 there is shown a plot detailing the activity for gold metal substrates having SAM applied to the surfaces of the electrode and including various functional groups.
  • the plots include both C-2 and C-11 length ligands.
  • the plots were generated utilizing the experimental apparatus described above with CO2 saturated 0.1M KHCO3 as an electrolyte at a pH of 6.8 at a constant potential of ⁇ 1.5 V and ⁇ 1.2V (vs. Ag/AgCl).
  • the ligand length, metal substrate and the choice of organic functional group may be selected to regulate the activity of the 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)
  • Inorganic Chemistry (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)
  • Chemical Treatment Of Metals (AREA)
US14/068,291 2013-10-31 2013-10-31 Surface modified electrodes for electrochemical syngas production Abandoned US20150114834A1 (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
US14/068,291 US20150114834A1 (en) 2013-10-31 2013-10-31 Surface modified electrodes for electrochemical syngas production
DE201410114658 DE102014114658A1 (de) 2013-10-31 2014-10-09 Oberflächenmodifizierte Elektroden für elektrochemische Synthesegasproduktion
CN201410539635.9A CN104593817B (zh) 2013-10-31 2014-10-14 用于生产电化学合成气的表面改性电极
JP2014218106A JP6485857B2 (ja) 2013-10-31 2014-10-27 電気化学的還元のための電極
US16/667,292 US20200063275A1 (en) 2013-10-31 2019-10-29 Surface modified electrodes for electrochemical syngas roduction

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104959135A (zh) * 2015-06-29 2015-10-07 华中师范大学 一种纳米锌催化剂及基于纳米锌催化剂高效催化co2还原co的方法
US10753003B2 (en) 2016-03-10 2020-08-25 Siemens Aktiengesellschaft Electrochemical production of synthesis gas

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CN108118361B (zh) * 2016-11-26 2019-05-21 中国科学院大连化学物理研究所 一种提高co2电化学还原用电极催化活性的方法
JP6902375B2 (ja) * 2017-03-29 2021-07-14 古河電気工業株式会社 銅系基材、並びにこれを用いた電極触媒および電解装置

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JP3009703B2 (ja) * 1990-05-02 2000-02-14 正道 藤平 二酸化炭素ガス還元用電極触媒
JP3949299B2 (ja) * 1998-11-05 2007-07-25 ペルメレック電極株式会社 酸素還元用電極及び該電極を使用する過酸化水素の製造方法
US7214331B2 (en) * 2004-02-26 2007-05-08 The Boc Group, Inc. Catalyst configuration and methods for syngas production
CN103227339B (zh) * 2007-04-03 2016-03-09 新空能量公司 产生可再生氢并截留二氧化碳的电化学系统、装置和方法
KR101762057B1 (ko) * 2013-05-29 2017-07-26 가부시끼가이샤 도시바 환원 촉매 및 화학 반응 장치

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104959135A (zh) * 2015-06-29 2015-10-07 华中师范大学 一种纳米锌催化剂及基于纳米锌催化剂高效催化co2还原co的方法
US10753003B2 (en) 2016-03-10 2020-08-25 Siemens Aktiengesellschaft Electrochemical production of synthesis gas

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US20200063275A1 (en) 2020-02-27
JP6485857B2 (ja) 2019-03-20
CN104593817A (zh) 2015-05-06
JP2015086472A (ja) 2015-05-07
CN104593817B (zh) 2019-06-04
DE102014114658A1 (de) 2015-05-13

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