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"Nano Lab" Advanced Characterization Platform for Studying Electrocatalytic Iridium Nanoparticles Dispersed on TiOxNy Supports Prepared on Ti Transmission Electron Microscopy Grids
Aiming at speeding up the discovery and understanding of promising electrocatalysts, a novel experimental platform, i.e. , the Nano Lab , is introduced. It is based on state-of-the-art physicochemical characterization and atomic-scale tracking of individual synthesis steps as well as subsequent elec...
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Published in: | ACS applied nano materials 2023-06, Vol.6 (12), p.10421-10430 |
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creator | Bele, Marjan Podboršek, Gorazd Koderman Lončar, Anja Jovanovič, Primož Hrnjić, Armin Marinko, Živa Kovač, Janez Surca, Angelja Kjara Kamšek, Ana Rebeka Dražić, Goran Hodnik, Nejc Suhadolnik, Luka |
description | Aiming at speeding up the discovery and understanding
of promising
electrocatalysts, a novel experimental platform,
i.e.
, the
Nano Lab
, is introduced. It is based on state-of-the-art
physicochemical characterization and atomic-scale tracking of individual
synthesis steps as well as subsequent electrochemical treatments targeting
nanostructured composites. This is provided by having the entire experimental
setup on a transmission electron microscopy (TEM) grid. Herein, the
oxygen evolution reaction nanocomposite electrocatalyst, i.e., iridium
nanoparticles dispersed on a high-surface-area TiO
x
N
y
support prepared on the Ti TEM
grid, is investigated. By combining electrochemical concepts such
as anodic oxidation of TEM grids, floating electrode-based electrochemical
characterization, and identical location TEM analysis, relevant information
from the entire composite’s cycle,
i.e.
, from
the initial synthesis step to electrochemical operation, can be studied.
We reveal that Ir nanoparticles as well as the TiO
x
N
y
support undergo dynamic changes
during all steps. The most interesting findings made possible by the
Nano Lab
concept are the formation of Ir single atoms and
only a small decrease in the N/O ratio of the TiO
x
N
y
–Ir catalyst during the
electrochemical treatment. In this way, we show that the precise influence
of the nanoscale structure, composition, morphology, and electrocatalyst’s
locally resolved surface sites can be deciphered on the atomic level.
Furthermore, the
Nano Lab
’s experimental setup
is compatible with
ex situ
characterization and other
analytical methods, such as Raman spectroscopy, X-ray photoelectron
spectroscopy, and identical location scanning electron microscopy,
hence providing a comprehensive understanding of structural changes
and their effects. Overall, an experimental toolbox for the systematic
development of supported electrocatalysts is now at hand. |
doi_str_mv | 10.1021/acsanm.3c01368 |
format | article |
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of promising
electrocatalysts, a novel experimental platform,
i.e.
, the
Nano Lab
, is introduced. It is based on state-of-the-art
physicochemical characterization and atomic-scale tracking of individual
synthesis steps as well as subsequent electrochemical treatments targeting
nanostructured composites. This is provided by having the entire experimental
setup on a transmission electron microscopy (TEM) grid. Herein, the
oxygen evolution reaction nanocomposite electrocatalyst, i.e., iridium
nanoparticles dispersed on a high-surface-area TiO
x
N
y
support prepared on the Ti TEM
grid, is investigated. By combining electrochemical concepts such
as anodic oxidation of TEM grids, floating electrode-based electrochemical
characterization, and identical location TEM analysis, relevant information
from the entire composite’s cycle,
i.e.
, from
the initial synthesis step to electrochemical operation, can be studied.
We reveal that Ir nanoparticles as well as the TiO
x
N
y
support undergo dynamic changes
during all steps. The most interesting findings made possible by the
Nano Lab
concept are the formation of Ir single atoms and
only a small decrease in the N/O ratio of the TiO
x
N
y
–Ir catalyst during the
electrochemical treatment. In this way, we show that the precise influence
of the nanoscale structure, composition, morphology, and electrocatalyst’s
locally resolved surface sites can be deciphered on the atomic level.
Furthermore, the
Nano Lab
’s experimental setup
is compatible with
ex situ
characterization and other
analytical methods, such as Raman spectroscopy, X-ray photoelectron
spectroscopy, and identical location scanning electron microscopy,
hence providing a comprehensive understanding of structural changes
and their effects. Overall, an experimental toolbox for the systematic
development of supported electrocatalysts is now at hand.</description><identifier>EISSN: 2574-0970</identifier><identifier>DOI: 10.1021/acsanm.3c01368</identifier><language>eng</language><publisher>American Chemical Society</publisher><ispartof>ACS applied nano materials, 2023-06, Vol.6 (12), p.10421-10430</ispartof><rights>2023 The Authors. Published by American Chemical Society 2023 The Authors</rights><lds50>peer_reviewed</lds50><oa>free_for_read</oa><woscitedreferencessubscribed>false</woscitedreferencessubscribed></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><link.rule.ids>230,315,786,790,891,27957,27958</link.rule.ids></links><search><creatorcontrib>Bele, Marjan</creatorcontrib><creatorcontrib>Podboršek, Gorazd Koderman</creatorcontrib><creatorcontrib>Lončar, Anja</creatorcontrib><creatorcontrib>Jovanovič, Primož</creatorcontrib><creatorcontrib>Hrnjić, Armin</creatorcontrib><creatorcontrib>Marinko, Živa</creatorcontrib><creatorcontrib>Kovač, Janez</creatorcontrib><creatorcontrib>Surca, Angelja Kjara</creatorcontrib><creatorcontrib>Kamšek, Ana Rebeka</creatorcontrib><creatorcontrib>Dražić, Goran</creatorcontrib><creatorcontrib>Hodnik, Nejc</creatorcontrib><creatorcontrib>Suhadolnik, Luka</creatorcontrib><title>"Nano Lab" Advanced Characterization Platform for Studying Electrocatalytic Iridium Nanoparticles Dispersed on TiOxNy Supports Prepared on Ti Transmission Electron Microscopy Grids</title><title>ACS applied nano materials</title><description>Aiming at speeding up the discovery and understanding
of promising
electrocatalysts, a novel experimental platform,
i.e.
, the
Nano Lab
, is introduced. It is based on state-of-the-art
physicochemical characterization and atomic-scale tracking of individual
synthesis steps as well as subsequent electrochemical treatments targeting
nanostructured composites. This is provided by having the entire experimental
setup on a transmission electron microscopy (TEM) grid. Herein, the
oxygen evolution reaction nanocomposite electrocatalyst, i.e., iridium
nanoparticles dispersed on a high-surface-area TiO
x
N
y
support prepared on the Ti TEM
grid, is investigated. By combining electrochemical concepts such
as anodic oxidation of TEM grids, floating electrode-based electrochemical
characterization, and identical location TEM analysis, relevant information
from the entire composite’s cycle,
i.e.
, from
the initial synthesis step to electrochemical operation, can be studied.
We reveal that Ir nanoparticles as well as the TiO
x
N
y
support undergo dynamic changes
during all steps. The most interesting findings made possible by the
Nano Lab
concept are the formation of Ir single atoms and
only a small decrease in the N/O ratio of the TiO
x
N
y
–Ir catalyst during the
electrochemical treatment. In this way, we show that the precise influence
of the nanoscale structure, composition, morphology, and electrocatalyst’s
locally resolved surface sites can be deciphered on the atomic level.
Furthermore, the
Nano Lab
’s experimental setup
is compatible with
ex situ
characterization and other
analytical methods, such as Raman spectroscopy, X-ray photoelectron
spectroscopy, and identical location scanning electron microscopy,
hence providing a comprehensive understanding of structural changes
and their effects. Overall, an experimental toolbox for the systematic
development of supported electrocatalysts is now at hand.</description><issn>2574-0970</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2023</creationdate><recordtype>article</recordtype><recordid>eNpVkUtLBDEQhAdBUNSr5-DJy67JPJOTyLo-YH2Aex96kp7dyEwyJhlx_F3-QCOuBy_d0NV8RVFJcsronNGUXYD0YPp5JinLSr6XHKZFlc-oqOhBcuL9K6WUCVZmlB4mX2ePYCxZQXNGrtQ7GImKLLbgQAZ0-hOCtoY8dxBa63oSB3kJo5q02ZBlhzI4KyFANwUtyb3TSo89-UEO4OKpQ0-utR_Q-ciNpLV--nicyMs4DNYFT54dxs8_jawdGN9r739cd3xDHrR01ks7TOQ2WvjjZL-FzuPJbh8l65vlenE3Wz3d3i-uVrOBCcFnOU8ZUlFg0xS8VU1FqWhFAYpJxnPZMpW3iFRWZVkwzLhkIs9bBpQ3FVcqO0ouf7HD2PSoJJrgoKsHp3twU21B1_8Vo7f1xr7XsQWRs7SKhPMdwdm3EX2oYzaJXQcG7ejrlGcsjb2URfYNn3qPiw</recordid><startdate>20230623</startdate><enddate>20230623</enddate><creator>Bele, Marjan</creator><creator>Podboršek, Gorazd Koderman</creator><creator>Lončar, Anja</creator><creator>Jovanovič, Primož</creator><creator>Hrnjić, Armin</creator><creator>Marinko, Živa</creator><creator>Kovač, Janez</creator><creator>Surca, Angelja Kjara</creator><creator>Kamšek, Ana Rebeka</creator><creator>Dražić, Goran</creator><creator>Hodnik, Nejc</creator><creator>Suhadolnik, Luka</creator><general>American Chemical Society</general><scope>7X8</scope><scope>5PM</scope></search><sort><creationdate>20230623</creationdate><title>"Nano Lab" Advanced Characterization Platform for Studying Electrocatalytic Iridium Nanoparticles Dispersed on TiOxNy Supports Prepared on Ti Transmission Electron Microscopy Grids</title><author>Bele, Marjan ; Podboršek, Gorazd Koderman ; Lončar, Anja ; Jovanovič, Primož ; Hrnjić, Armin ; Marinko, Živa ; Kovač, Janez ; Surca, Angelja Kjara ; Kamšek, Ana Rebeka ; Dražić, Goran ; Hodnik, Nejc ; Suhadolnik, Luka</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-p1998-4821e095ebb58fdb7009f95ad1c184cf1d4fee0c76651e38c1944f1a08b78dd3</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2023</creationdate><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Bele, Marjan</creatorcontrib><creatorcontrib>Podboršek, Gorazd Koderman</creatorcontrib><creatorcontrib>Lončar, Anja</creatorcontrib><creatorcontrib>Jovanovič, Primož</creatorcontrib><creatorcontrib>Hrnjić, Armin</creatorcontrib><creatorcontrib>Marinko, Živa</creatorcontrib><creatorcontrib>Kovač, Janez</creatorcontrib><creatorcontrib>Surca, Angelja Kjara</creatorcontrib><creatorcontrib>Kamšek, Ana Rebeka</creatorcontrib><creatorcontrib>Dražić, Goran</creatorcontrib><creatorcontrib>Hodnik, Nejc</creatorcontrib><creatorcontrib>Suhadolnik, Luka</creatorcontrib><collection>MEDLINE - Academic</collection><collection>PubMed Central (Full Participant titles)</collection><jtitle>ACS applied nano materials</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Bele, Marjan</au><au>Podboršek, Gorazd Koderman</au><au>Lončar, Anja</au><au>Jovanovič, Primož</au><au>Hrnjić, Armin</au><au>Marinko, Živa</au><au>Kovač, Janez</au><au>Surca, Angelja Kjara</au><au>Kamšek, Ana Rebeka</au><au>Dražić, Goran</au><au>Hodnik, Nejc</au><au>Suhadolnik, Luka</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>"Nano Lab" Advanced Characterization Platform for Studying Electrocatalytic Iridium Nanoparticles Dispersed on TiOxNy Supports Prepared on Ti Transmission Electron Microscopy Grids</atitle><jtitle>ACS applied nano materials</jtitle><date>2023-06-23</date><risdate>2023</risdate><volume>6</volume><issue>12</issue><spage>10421</spage><epage>10430</epage><pages>10421-10430</pages><eissn>2574-0970</eissn><notes>ObjectType-Article-1</notes><notes>SourceType-Scholarly Journals-1</notes><notes>ObjectType-Feature-2</notes><notes>content type line 23</notes><abstract>Aiming at speeding up the discovery and understanding
of promising
electrocatalysts, a novel experimental platform,
i.e.
, the
Nano Lab
, is introduced. It is based on state-of-the-art
physicochemical characterization and atomic-scale tracking of individual
synthesis steps as well as subsequent electrochemical treatments targeting
nanostructured composites. This is provided by having the entire experimental
setup on a transmission electron microscopy (TEM) grid. Herein, the
oxygen evolution reaction nanocomposite electrocatalyst, i.e., iridium
nanoparticles dispersed on a high-surface-area TiO
x
N
y
support prepared on the Ti TEM
grid, is investigated. By combining electrochemical concepts such
as anodic oxidation of TEM grids, floating electrode-based electrochemical
characterization, and identical location TEM analysis, relevant information
from the entire composite’s cycle,
i.e.
, from
the initial synthesis step to electrochemical operation, can be studied.
We reveal that Ir nanoparticles as well as the TiO
x
N
y
support undergo dynamic changes
during all steps. The most interesting findings made possible by the
Nano Lab
concept are the formation of Ir single atoms and
only a small decrease in the N/O ratio of the TiO
x
N
y
–Ir catalyst during the
electrochemical treatment. In this way, we show that the precise influence
of the nanoscale structure, composition, morphology, and electrocatalyst’s
locally resolved surface sites can be deciphered on the atomic level.
Furthermore, the
Nano Lab
’s experimental setup
is compatible with
ex situ
characterization and other
analytical methods, such as Raman spectroscopy, X-ray photoelectron
spectroscopy, and identical location scanning electron microscopy,
hence providing a comprehensive understanding of structural changes
and their effects. Overall, an experimental toolbox for the systematic
development of supported electrocatalysts is now at hand.</abstract><pub>American Chemical Society</pub><doi>10.1021/acsanm.3c01368</doi><tpages>10</tpages><oa>free_for_read</oa></addata></record> |
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language | eng |
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title | "Nano Lab" Advanced Characterization Platform for Studying Electrocatalytic Iridium Nanoparticles Dispersed on TiOxNy Supports Prepared on Ti Transmission Electron Microscopy Grids |
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