Direct atomic-level insight into the active sites of a high-performance PGM-free ORR catalyst

Chung, Hoon T.; Cullen, David A.; Higgins, Drew; Sneed, Brian T.; Holby, Edward F.; More, Karren L.; Zelenay, Piotr

doi:10.1126/science.aan2255

Title: Direct atomic-level insight into the active sites of a high-performance PGM-free ORR catalyst

Journal Article · 03 August 2017 · Science

DOI: https://doi.org/10.1126/science.aan2255 · OSTI ID:1376619

^[1];

^[2]; Higgins, Drew ^[1];

^[2];

^[1]; More, Karren L. ^[2];

^[1]

Los Alamos National Lab. (LANL), Los Alamos, NM (United States)
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

Platinum group metal–free (PGM-free) metal-nitrogen-carbon catalysts have emerged as a promising alternative to their costly platinum (Pt)–based counterparts in polymer electrolyte fuel cells (PEFCs) but still face some major challenges, including (i) the identification of the most relevant catalytic site for the oxygen reduction reaction (ORR) and (ii) demonstration of competitive PEFC performance under automotive-application conditions in the hydrogen (H₂)–air fuel cell. We demonstrate H₂-air performance gains achieved with an iron-nitrogen-carbon catalyst synthesized with two nitrogen precursors that developed hierarchical porosity. In current densities recorded in the kinetic region of cathode operation, at fuel cell voltages greater than ~0.75 V, were the same as those obtained with a Pt cathode at a loading of 0.1 milligram of Pt per centimeter squared. The catalytic active site we proposed, carbon-embedded nitrogen-coordinated iron (FeN₄), was directly visualized with aberration-corrected scanning transmission electron microscopy, and the contributions of these active sites associated with specific lattice-level carbon structures were explored computationally.

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Research Organization:: Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)

Sponsoring Organization:: USDOE Office of Energy Efficiency and Renewable Energy (EERE), Fuel Cell Technologies Program (EE-3F)

Grant/Contract Number:: AC05-00OR22725

OSTI ID:: 1376619

Alternate ID(s):: OSTI ID: 1458952

Journal Information:: Science, Journal Name: Science Journal Issue: 6350 Vol. 357; ISSN 0036-8075

Publisher:: AAASCopyright Statement

Country of Publication:: United States

Language:: English

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Lattice-strained metal–organic-framework arrays for bifunctional oxygen electrocatalysis Cheng, Weiren; Zhao, Xu; Su, Hui Nature Energy, Vol. 4, Issue 2 https://doi.org/10.1038/s41560-018-0308-8	journal	January 2019
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Carbon-Supported Single Atom Catalysts for Electrochemical Energy Conversion and Storage Peng, Yi; Lu, Bingzhang; Chen, Shaowei Advanced Materials, Vol. 30, Issue 48 https://doi.org/10.1002/adma.201801995	journal	August 2018
Optimal coordination-site exposure engineering in porous platinum for outstanding oxygen reduction performance Cheng, Han; Liu, Si; Hao, Zikai Chemical Science, Vol. 10, Issue 21 https://doi.org/10.1039/c9sc01078e	journal	January 2019
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Atomic-level active sites of efficient imidazolate framework-derived nickel catalysts for CO ₂ reduction Pan, Fuping; Zhang, Hanguang; Liu, Zhenyu Journal of Materials Chemistry A, Vol. 7, Issue 46 https://doi.org/10.1039/c9ta08862h	journal	January 2019
Electrochemical Evidence for Two Sub-families of FeN _x C _y Moieties with Concentration-Dependent Cyanide Poisoning Chung, Min Wook; Chon, Gajeon; Kim, Hyungjun ChemElectroChem, Vol. 5, Issue 14 https://doi.org/10.1002/celc.201800067	journal	March 2018
An Oxygen‐Vacancy‐Rich Semiconductor‐Supported Bifunctional Catalyst for Efficient and Stable Zinc–Air Batteries Liu, Guihua; Li, Jingde; Fu, Jing Advanced Materials https://doi.org/10.1002/adma.201806761	journal	December 2018
Design strategies for developing non-precious metal based bi-functional catalysts for alkaline electrolyte based zinc–air batteries Han, Chao; Li, Weijie; Liu, Hua-Kun Materials Horizons, Vol. 6, Issue 9 https://doi.org/10.1039/c9mh00502a	journal	January 2019
Molecular Design of Single‐Atom Catalysts for Oxygen Reduction Reaction Wan, Chengzhang; Duan, Xiangfeng; Huang, Yu Advanced Energy Materials, Vol. 10, Issue 14 https://doi.org/10.1002/aenm.201903815	journal	February 2020
An Fe–N co-doped tube-in-tube carbon nanostructure used as an efficient catalyst for the electrochemical oxygen reduction reaction Zhang, Jianshuo; Zhao, Yi; Hou, Kun Nanotechnology, Vol. 30, Issue 48 https://doi.org/10.1088/1361-6528/ab3ceb	journal	September 2019
Metal–organic frameworks: a promising platform for constructing non-noble electrocatalysts for the oxygen-reduction reaction Li, Liangjun; He, Jiangxiu; Wang, Ying Journal of Materials Chemistry A, Vol. 7, Issue 5 https://doi.org/10.1039/c8ta11704g	journal	January 2019
The Role of Supported Atomically Distributed Metal Species in Electrochemistry and How to Create Them Ding, Yuxiao; Schlögl, Robert; Heumann, Saskia ChemElectroChem, Vol. 6, Issue 15 https://doi.org/10.1002/celc.201900598	journal	May 2019
A pyrolysis-free path toward superiorly catalytic nitrogen-coordinated single atom Peng, Peng; Shi, Lei; Huo, Feng Science Advances, Vol. 5, Issue 8 https://doi.org/10.1126/sciadv.aaw2322	journal	August 2019
In Situ and Operando Characterization of Proton Exchange Membrane Fuel Cells Meyer, Quentin; Zeng, Yachao; Zhao, Chuan Advanced Materials, Vol. 31, Issue 40 https://doi.org/10.1002/adma.201901900	journal	August 2019
Toward Efficient Carbon and Water Cycles: Emerging Opportunities with Single‐Site Catalysts Made of 3d Transition Metals Wan, Gang; Zhang, Guanghui; Lin, Xiao‐Min Advanced Materials, Vol. 32, Issue 2 https://doi.org/10.1002/adma.201905548	journal	November 2019
N,S-Atom-coordinated Co ₉ S ₈ trinary dopants within a porous graphene framework as efficient catalysts for oxygen reduction/evolution reactions Li, Yi; Zhou, Yazhou; Wen, Hejing Dalton Transactions, Vol. 47, Issue 42 https://doi.org/10.1039/c8dt02324g	journal	January 2018
Dynamic oxygen adsorption on single-atomic Ruthenium catalyst with high performance for acidic oxygen evolution reaction Cao, Linlin; Luo, Qiquan; Chen, Jiajia Nature Communications, Vol. 10, Issue 1 https://doi.org/10.1038/s41467-019-12886-z	journal	October 2019
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Synthesis and Active Site Identification of Fe−N−C Single-Atom Catalysts for the Oxygen Reduction Reaction Wan, Xin; Chen, Weiqi; Yang, Jiarui ChemElectroChem, Vol. 6, Issue 2 https://doi.org/10.1002/celc.201801302	journal	November 2018
Engineering Single-Atom Cobalt Catalysts toward Improved Electrocatalysis Wan, Gang; Yu, Pengfei; Chen, Hangrong Small, Vol. 14, Issue 15 https://doi.org/10.1002/smll.201704319	journal	March 2018
Transition Metal‐Nitrogen‐Carbon Active Site for Oxygen Reduction Electrocatalysis: Beyond the Fascinations of TM‐N₄ Zhang, Cai; Zhang, Wei; Zheng, Weitao ChemCatChem, Vol. 11, Issue 2 https://doi.org/10.1002/cctc.201801679	journal	November 2018
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Hierarchically Porous M-N-C (M = Co and Fe) Single-Atom Electrocatalysts with Robust MN _x Active Moieties Enable Enhanced ORR Performance Zhu, Chengzhou; Shi, Qiurong; Xu, Bo Z. Advanced Energy Materials, Vol. 8, Issue 29 https://doi.org/10.1002/aenm.201801956	journal	August 2018
Rational design of electrocatalysts and photo(electro)catalysts for nitrogen reduction to ammonia (NH ₃ ) under ambient conditions Guo, Chunxian; Ran, Jingrun; Vasileff, Anthony Energy & Environmental Science, Vol. 11, Issue 1 https://doi.org/10.1039/c7ee02220d	journal	January 2018
Analysis of the effect of catalyst layer thickness on the performance and durability of platinum group metal-free catalysts for polymer electrolyte membrane fuel cells Baricci, Andrea; Bisello, Andrea; Serov, Alexey Sustainable Energy & Fuels, Vol. 3, Issue 12 https://doi.org/10.1039/c9se00252a	journal	January 2019
ORR Activity and Stability of Co-N/C Catalysts Based on Silicon Carbide Derived Carbon and the Impact of Loading in Acidic Media Teppor, P.; Jäger, R.; Härk, E. Journal of The Electrochemical Society, Vol. 165, Issue 14 https://doi.org/10.1149/2.0961814jes	journal	January 2018
Carbon-Rich Nanomaterials: Fascinating Hydrogen and Oxygen Electrocatalysts Zhang, Jian; Chen, Guangbo; Müllen, Klaus Advanced Materials, Vol. 30, Issue 40 https://doi.org/10.1002/adma.201800528	journal	July 2018
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High-performance Platinum-free oxygen reduction reaction and hydrogen oxidation reaction catalyst in polymer electrolyte membrane fuel cell Chandran, Priji; Ghosh, Arpita; Ramaprabhu, Sundara Scientific Reports, Vol. 8, Issue 1 https://doi.org/10.1038/s41598-018-22001-9	journal	February 2018
Hierarchically porous Fe/N–C hollow spheres derived from melamine/Fe-incorporated polydopamine for efficient oxygen reduction reaction electrocatalysis Feng, Bomin; Wu, Xiuju; Niu, Yanli Sustainable Energy & Fuels, Vol. 3, Issue 12 https://doi.org/10.1039/c9se00686a	journal	January 2019
Standing Carbon‐Supported Trace Levels of Metal Derived from Covalent Organic Framework for Electrocatalysis Xu, Qing; Zhang, Hao; Guo, Yu Small, Vol. 15, Issue 50 https://doi.org/10.1002/smll.201905363	journal	October 2019
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The Sub-Nanometer Scale as a New Focus in Nanoscience Ni, Bing; Shi, Yuang; Wang, Xun Advanced Materials, Vol. 30, Issue 43 https://doi.org/10.1002/adma.201802031	journal	July 2018
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The Role of Polyaniline Molecular Structure in Producing High‐Performance Fe‐N‐C Catalysts for Oxygen Reduction Reaction He, Qian; Chen, Xiuhong; Jia, Fengqiu ChemistrySelect, Vol. 4, Issue 27 https://doi.org/10.1002/slct.201901329	journal	July 2019
High-purity pyrrole-type FeN ₄ sites as a superior oxygen reduction electrocatalyst Zhang, Nan; Zhou, Tianpei; Chen, Minglong Energy & Environmental Science, Vol. 13, Issue 1 https://doi.org/10.1039/c9ee03027a	journal	January 2020
Heterogeneous Single Atom Electrocatalysis, Where “Singles” Are “Married” Zang, Wenjie; Kou, Zongkui; Pennycook, Stephen J. Advanced Energy Materials, Vol. 10, Issue 9 https://doi.org/10.1002/aenm.201903181	journal	January 2020
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Bioinspired Transition‐Metal Complexes as Electrocatalysts for the Oxygen Reduction Reaction Zhao, Ye‐Min; Yu, Guo‐Qiang; Wang, Fei‐Fei Chemistry – A European Journal, Vol. 25, Issue 15 https://doi.org/10.1002/chem.201803764	journal	December 2018
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Understanding Degradation and Active Sites in Nitrogen-Doped Carbon Nanotube-Based Electrocatalysts Chen, Ti; Takahashi, Shota; Fukushima, Yomei Journal of The Electrochemical Society, Vol. 166, Issue 2 https://doi.org/10.1149/2.0781902jes	journal	January 2019
A specific demetalation of Fe–N ₄ catalytic sites in the micropores of NC_Ar + NH ₃ is at the origin of the initial activity loss of the highly active Fe/N/C catalyst used for the reduction of oxygen in PEM fuel cells Chenitz, Régis; Kramm, Ulrike I.; Lefèvre, Michel Energy & Environmental Science, Vol. 11, Issue 2 https://doi.org/10.1039/c7ee02302b	journal	January 2018
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Confinement Catalysis with 2D Materials for Energy Conversion Tang, Lei; Meng, Xianguang; Deng, Dehui Advanced Materials, Vol. 31, Issue 50 https://doi.org/10.1002/adma.201901996	journal	July 2019
Iron Single Atoms on Graphene as Nonprecious Metal Catalysts for High‐Temperature Polymer Electrolyte Membrane Fuel Cells Cheng, Yi; He, Shuai; Lu, Shanfu Advanced Science, Vol. 6, Issue 10 https://doi.org/10.1002/advs.201802066	journal	March 2019
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The Achilles' heel of iron-based catalysts during oxygen reduction in an acidic medium Choi, Chang Hyuck; Lim, Hyung-Kyu; Chung, Min Wook Energy & Environmental Science, Vol. 11, Issue 11 https://doi.org/10.1039/c8ee01855c	journal	January 2018
Progress in the Development of Fe‐Based PGM‐Free Electrocatalysts for the Oxygen Reduction Reaction Martinez, Ulises; Komini Babu, Siddharth; Holby, Edward F. Advanced Materials, Vol. 31, Issue 31 https://doi.org/10.1002/adma.201806545	journal	December 2018
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N‐Doped Graphene Supported on Metal‐Iron Carbide as a Catalyst for the Oxygen Reduction Reaction: Density Functional Theory Study Patniboon, Tipaporn; Hansen, Heine Anton ChemSusChem, Vol. 13, Issue 5 https://doi.org/10.1002/cssc.201903035	journal	January 2020
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Ambient Synthesis of Single‐Atom Catalysts from Bulk Metal via Trapping of Atoms by Surface Dangling Bonds Qu, Yunteng; Wang, Liguang; Li, Zhijun Advanced Materials, Vol. 31, Issue 44 https://doi.org/10.1002/adma.201904496	journal	September 2019
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Structure of Active Sites of Fe-N-C Nano-Catalysts for Alkaline Exchange Membrane Fuel Cells Kishi, Hirofumi; Sakamoto, Tomokazu; Asazawa, Koichiro Nanomaterials, Vol. 8, Issue 12 https://doi.org/10.3390/nano8120965	journal	November 2018
An active oxygen reduction electrocatalyst derived from bio-inspired tannic acid-Fe assembly Chen, Chan; Zhang, Zhijia; Yin, Yaqing Materials Research Express, Vol. 5, Issue 9 https://doi.org/10.1088/2053-1591/aad601	journal	August 2018
Nitrogen-doped Carbon-CoO _x Nanohybrids: A Precious Metal Free Cathode that Exceeds 1.0 W cm ⁻² Peak Power and 100 h Life in Anion-Exchange Membrane Fuel Cells Peng, Xiong; Omasta, Travis J.; Magliocca, Emanuele Angewandte Chemie International Edition, Vol. 58, Issue 4 https://doi.org/10.1002/anie.201811099	journal	November 2018
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Fe2N nanoparticles boosting FeNx moieties for highly efficient oxygen reduction reaction in Fe-N-C porous catalyst Liu, Xiao; Liu, Hong; Chen, Chi Nano Research, Vol. 12, Issue 7 https://doi.org/10.1007/s12274-019-2415-7	journal	April 2019
Zirconium nitride catalysts surpass platinum for oxygen reduction Yuan, Yao; Wang, Jiacheng; Adimi, Samira Nature Materials, Vol. 19, Issue 3 https://doi.org/10.1038/s41563-019-0535-9	journal	November 2019
A ZIF-derived hierarchically porous Fe–Zn–N–C catalyst synthesized via a two-stage pyrolysis for the highly efficient oxygen reduction reaction in both acidic and alkaline media Li, Fang; Ding, Xiao-Bo; Cao, Qing-Cheng Chemical Communications, Vol. 55, Issue 93 https://doi.org/10.1039/c9cc07489a	journal	January 2019
Optimal coordination-site exposure engineering in porous platinum for outstanding oxygen reduction performance Cheng, Han; Liu, Si; Hao, Zikai Chemical Science, Vol. 10, Issue 21 https://doi.org/10.1039/c9sc01078e	journal	January 2019
Iron Phosphide Incorporated into Iron-Treated Heteroatoms-Doped Porous Bio-Carbon as Efficient Electrocatalyst for the Oxygen Reduction Reaction Tran, Thanh-Nhan; Song, Min Young; Kang, Tong-Hyun ChemElectroChem, Vol. 5, Issue 14 https://doi.org/10.1002/celc.201800091	journal	April 2018
Advanced Architectures and Relatives of Air Electrodes in Zn-Air Batteries Pan, Jing; Xu, Yang Yang; Yang, Huan Advanced Science, Vol. 5, Issue 4 https://doi.org/10.1002/advs.201700691	journal	January 2018
Fabrication of Superior Single‐Atom Catalysts toward Diverse Electrochemical Reactions Zhang, Bin‐Wei; Wang, Yun‐Xiao; Chou, Shu‐Lei Small Methods, Vol. 3, Issue 9 https://doi.org/10.1002/smtd.201800497	journal	February 2019
A Review on Recent Progress in the Aspect of Stability of Oxygen Reduction Electrocatalysts for Proton‐Exchange Membrane Fuel Cell: Quantum Mechanics and Experimental Approaches Lee, Jong Min; Han, Hyunsu; Jin, Song Energy Technology, Vol. 7, Issue 9 https://doi.org/10.1002/ente.201900312	journal	June 2019
PtRu/C catalyst slurry preparation for large-scale decal transfer with high performance of proton exchange membrane fuel cells Choi, Mihwa; Kim, Jong Kwan; Kim, Jungsuk RSC Advances, Vol. 8, Issue 63 https://doi.org/10.1039/c8ra07754a	journal	January 2018
Atomic-level tuning of Co–N–C catalyst for high-performance electrochemical H2O2 production Jung, Euiyeon; Shin, Heejong; Lee, Byoung-Hoon Nature Materials, Vol. 19, Issue 4 https://doi.org/10.1038/s41563-019-0571-5	journal	January 2020
Electronic structure engineering to boost oxygen reduction activity by controlling the coordination of the central metal Han, Yunhu; Wang, Yanggang; Xu, Ruirui Energy & Environmental Science, Vol. 11, Issue 9 https://doi.org/10.1039/c8ee01481g	journal	January 2018
Zinc‐Mediated Template Synthesis of Fe‐N‐C Electrocatalysts with Densely Accessible Fe‐N _x Active Sites for Efficient Oxygen Reduction Chen, Guangbo; Liu, Pan; Liao, Zhongquan Advanced Materials, Vol. 32, Issue 8 https://doi.org/10.1002/adma.201907399	journal	January 2020
Ultranarrow Graphene Nanoribbons toward Oxygen Reduction and Evolution Reactions Zhang, Jian; Sun, Yuanmiao; Zhu, Jiawei Advanced Science, Vol. 5, Issue 12 https://doi.org/10.1002/advs.201801375	journal	November 2018
Dynamic oxygen adsorption on single-atomic Ruthenium catalyst with high performance for acidic oxygen evolution reaction Cao, Linlin; Luo, Qiquan; Chen, Jiajia Nature Communications, Vol. 10, Issue 1 https://doi.org/10.1038/s41467-019-12886-z	journal	October 2019
Non-PGM Electrocatalysts for PEM Fuel Cells: Thermodynamic Stability and DFT Evaluation of Fluorinated FeN ₄ -Based ORR Catalysts Glibin, Vassili P.; Cherif, Mohamed; Vidal, François Journal of The Electrochemical Society, Vol. 166, Issue 7 https://doi.org/10.1149/2.0341907jes	journal	January 2019
Less active CeO ₂ regulating bifunctional oxygen electrocatalytic activity of Co ₃ O ₄ @N-doped carbon for Zn–air batteries He, Xiaobo; Yi, Xuerui; Yin, Fengxiang Journal of Materials Chemistry A, Vol. 7, Issue 12 https://doi.org/10.1039/c9ta00302a	journal	January 2019
Electroreduction of CO ₂ on Single‐Site Copper‐Nitrogen‐Doped Carbon Material: Selective Formation of Ethanol and Reversible Restructuration of the Metal Sites Karapinar, Dilan; Huan, Ngoc Tran; Ranjbar Sahraie, Nastaran Angewandte Chemie, Vol. 131, Issue 42 https://doi.org/10.1002/ange.201907994	journal	September 2019
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Tailoring the Electrochemical Production of H ₂ O ₂ : Strategies for the Rational Design of High‐Performance Electrocatalysts Zhang, Jiayi; Zhang, Haochen; Cheng, Mu‐Jeng Small, Vol. 16, Issue 15 https://doi.org/10.1002/smll.201902845	journal	September 2019
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Nitrogen‐doped Carbon–CoO _x Nanohybrids: A Precious Metal Free Cathode that Exceeds 1.0 W cm ⁻² Peak Power and 100 h Life in Anion‐Exchange Membrane Fuel Cells Peng, Xiong; Omasta, Travis J.; Magliocca, Emanuele Angewandte Chemie, Vol. 131, Issue 4 https://doi.org/10.1002/ange.201811099	journal	November 2018
Investigation of Earth-Abundant Oxygen Reduction Electrocatalysts for the Cathode of Passive Air-Breathing Direct Formate Fuel Cells E. R. Oliveira, Francisca; A. Galiote, Nelson; H. B. Lima, Fabio Catalysts, Vol. 8, Issue 8 https://doi.org/10.3390/catal8080320	journal	August 2018
Cascade anchoring strategy for general mass production of high-loading single-atomic metal-nitrogen catalysts Zhao, Lu; Zhang, Yun; Huang, Lin-Bo Nature Communications, Vol. 10, Issue 1 https://doi.org/10.1038/s41467-019-09290-y	journal	March 2019

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