The University of Southampton
University of Southampton Institutional Repository

The electronic structure, surface properties, and in situ N2O decomposition of mechanochemically synthesised LaMnO3

The electronic structure, surface properties, and in situ N2O decomposition of mechanochemically synthesised LaMnO3
The electronic structure, surface properties, and in situ N2O decomposition of mechanochemically synthesised LaMnO3
The use of mechanochemistry to prepare catalytic materials is of significant interest; it offers an environmentally beneficial, solvent-free, route and produces highly complex structures of mixed amorphous and crystalline phases. This study reports on the effect of milling atmosphere, either air or argon, on mechanochemically prepared LaMnO3 and the catalytic performance towards N2O decomposition (deN2O). In this work, high energy resolution fluorescence detection (HERFD), X-ray absorption near edge structure (XANES), X-ray emission, and X-ray photoelectron spectroscopy (XPS) have been used to probe the electronic structural properties of the mechanochemically prepared materials. Moreover, in situ studies using near ambient pressure (NAP)-XPS, to follow the materials during catalysis, and high pressure energy dispersive EXAFS studies, to mimic the preparation conditions, have also been performed. The studies show that there are clear differences between the air and argon milled samples, with the most pronounced changes observed using NAP-XPS. The XPS results find increased levels of active adsorbed oxygen species, linked to the presence of surface oxide vacancies, for the sample prepared in argon. Furthermore, the argon milled LaMnO3 shows improved catalytic activity towards deN2O at lower temperatures compared to the air milled and sol–gel synthesised LaMnO3. Assessing this improved catalytic behaviour during deN2O of argon milled LaMnO3 by in situ NAP-XPS suggests increased interaction of N2O at room temperature within the O 1s region. This study further demonstrates the complexity of mechanochemically prepared materials and through careful choice of characterisation methods how their properties can be understood.
1463-9076
18774-18787
Blackmore, Rachel Hazel
3584b852-92ac-4341-b303-786f67e41f77
Rivas, Maria Elena
08dfefa0-544f-4c89-a1c8-7a58560a59e1
Tierney, George
5a1b1e97-5868-4933-a321-9b2cdfb69c5a
Mohammed, Khaled Mohammed Hassan
f50a275b-4588-43b0-ba9c-5f108f23d3fc
Decarolis, Donato
aa002823-ac92-4afe-aa03-83562110dd3c
Hayama, Shusaku
dbaecfbe-b0a6-4b21-9030-b2942d42b33c
Venturini, Federica
a4ddd918-9bbf-450a-b8e6-558d30301bb2
Held, Georg
ad070380-ba97-42db-9a0d-9e5d73b62cd0
Arrigo, Rosa
0998a17a-56f9-49c6-8a47-bdd9099c523a
Amboage, Monica
f1f91840-c149-4732-b396-0c20e11aaeb6
Hellier, Pip
c3bd090a-2f8d-45ec-8ee6-781c034eb9b9
Lynch, Evan William
6eecfe8a-33be-44bb-9498-e1d378d526ff
Amri, Mahrez
e468ed70-db5e-447f-a174-8afa413922af
Casavola, Marianna
a5a1b50c-6fa4-40e8-a155-9df4426f60cd
Erden, Tugce Eralp
758531fc-bdd2-4122-bc1b-2e4438b1a282
Collier, Paul
35e8d4e9-9569-48f9-9e98-43076647796e
Wells, Peter P.
bc4fdc2d-a490-41bf-86cc-400edecf2266
Blackmore, Rachel Hazel
3584b852-92ac-4341-b303-786f67e41f77
Rivas, Maria Elena
08dfefa0-544f-4c89-a1c8-7a58560a59e1
Tierney, George
5a1b1e97-5868-4933-a321-9b2cdfb69c5a
Mohammed, Khaled Mohammed Hassan
f50a275b-4588-43b0-ba9c-5f108f23d3fc
Decarolis, Donato
aa002823-ac92-4afe-aa03-83562110dd3c
Hayama, Shusaku
dbaecfbe-b0a6-4b21-9030-b2942d42b33c
Venturini, Federica
a4ddd918-9bbf-450a-b8e6-558d30301bb2
Held, Georg
ad070380-ba97-42db-9a0d-9e5d73b62cd0
Arrigo, Rosa
0998a17a-56f9-49c6-8a47-bdd9099c523a
Amboage, Monica
f1f91840-c149-4732-b396-0c20e11aaeb6
Hellier, Pip
c3bd090a-2f8d-45ec-8ee6-781c034eb9b9
Lynch, Evan William
6eecfe8a-33be-44bb-9498-e1d378d526ff
Amri, Mahrez
e468ed70-db5e-447f-a174-8afa413922af
Casavola, Marianna
a5a1b50c-6fa4-40e8-a155-9df4426f60cd
Erden, Tugce Eralp
758531fc-bdd2-4122-bc1b-2e4438b1a282
Collier, Paul
35e8d4e9-9569-48f9-9e98-43076647796e
Wells, Peter P.
bc4fdc2d-a490-41bf-86cc-400edecf2266

Blackmore, Rachel Hazel, Rivas, Maria Elena, Tierney, George, Mohammed, Khaled Mohammed Hassan, Decarolis, Donato, Hayama, Shusaku, Venturini, Federica, Held, Georg, Arrigo, Rosa, Amboage, Monica, Hellier, Pip, Lynch, Evan William, Amri, Mahrez, Casavola, Marianna, Erden, Tugce Eralp, Collier, Paul and Wells, Peter P. (2020) The electronic structure, surface properties, and in situ N2O decomposition of mechanochemically synthesised LaMnO3. Physical Chemistry Chemical Physics, 22 (34), 18774-18787. (doi:10.1039/D0CP00793E).

Record type: Article

Abstract

The use of mechanochemistry to prepare catalytic materials is of significant interest; it offers an environmentally beneficial, solvent-free, route and produces highly complex structures of mixed amorphous and crystalline phases. This study reports on the effect of milling atmosphere, either air or argon, on mechanochemically prepared LaMnO3 and the catalytic performance towards N2O decomposition (deN2O). In this work, high energy resolution fluorescence detection (HERFD), X-ray absorption near edge structure (XANES), X-ray emission, and X-ray photoelectron spectroscopy (XPS) have been used to probe the electronic structural properties of the mechanochemically prepared materials. Moreover, in situ studies using near ambient pressure (NAP)-XPS, to follow the materials during catalysis, and high pressure energy dispersive EXAFS studies, to mimic the preparation conditions, have also been performed. The studies show that there are clear differences between the air and argon milled samples, with the most pronounced changes observed using NAP-XPS. The XPS results find increased levels of active adsorbed oxygen species, linked to the presence of surface oxide vacancies, for the sample prepared in argon. Furthermore, the argon milled LaMnO3 shows improved catalytic activity towards deN2O at lower temperatures compared to the air milled and sol–gel synthesised LaMnO3. Assessing this improved catalytic behaviour during deN2O of argon milled LaMnO3 by in situ NAP-XPS suggests increased interaction of N2O at room temperature within the O 1s region. This study further demonstrates the complexity of mechanochemically prepared materials and through careful choice of characterisation methods how their properties can be understood.

Text
PCCP_AFTER_ACCEPTANCE_REVISIONS_UNMARKED.RB_PW - Accepted Manuscript
Available under License Creative Commons Attribution.
Download (1MB)

More information

Accepted/In Press date: 7 April 2020
e-pub ahead of print date: 30 June 2020
Published date: 14 September 2020
Additional Information: Funding Information: The authors acknowledge Diamond Light Source for provision of beamtimes (experiments SP20129, SP20200 and SP22063) along with the UK Catalysis Hub for provision of beamtime SP15151-8. The staff on B18, I20-Scanning, I20-EDE and B07-C at Diamond Light Source are thanked. Particularly Dr Diego Gianolio is thanked for his assistance in collecting data on B18 and Dave Grinter, Pilar Ferrer-Escorihuela and Rosa Arrigo for establishing the B07-C beamline. Also, to the ID15A beamline and their staff at the European Synchrotron Radiation Facility and particularly to the Rud-er BoˇskovićInstitute for the use of their in situ milling set-up (experiment CH-5331). The RCaH are acknowledged for use of facilities and staff support. Johnson Matthey is acknowledged for their provision of precursor materials and milling equipment. The Johnson Matthey advanced analytical department are also thanked for their help and support throughout the project. The UK Catalysis Hub is kindly thanked for resources and support provided via our membership of the UK Catalysis Hub Consortium (portfolio grants EP//K014706/1, EP/K014668/1, EP/K014854/1, EP/K014714/1 and EP/I019693/1). The University of Southampton and EPSRC are thanked for the iCASE studentship of RHB. PW and KM wish to acknowledge the STFC for funding the position of KM (ST/R002754/1). PW and MC wish to acknowledge the EPSRC for funding the position of MC (EP/R011710/1). All data supporting this study are openly available from the University of Southampton repository at DOI: 10.5258/ SOTON/D1342. Publisher Copyright: © 2010 the Owner Societies.

Identifiers

Local EPrints ID: 442910
URI: http://eprints.soton.ac.uk/id/eprint/442910
ISSN: 1463-9076
PURE UUID: ca48923c-f962-4c27-8a4d-4493cbb07aed
ORCID for Evan William Lynch: ORCID iD orcid.org/0009-0007-6799-7457
ORCID for Marianna Casavola: ORCID iD orcid.org/0000-0002-8902-7431
ORCID for Peter P. Wells: ORCID iD orcid.org/0000-0002-0859-9172

Catalogue record

Date deposited: 31 Jul 2020 16:30
Last modified: 06 Jun 2024 02:03

Export record

Altmetrics

Contributors

Author: Rachel Hazel Blackmore
Author: Maria Elena Rivas
Author: George Tierney
Author: Khaled Mohammed Hassan Mohammed
Author: Donato Decarolis
Author: Shusaku Hayama
Author: Federica Venturini
Author: Georg Held
Author: Rosa Arrigo
Author: Monica Amboage
Author: Pip Hellier
Author: Evan William Lynch ORCID iD
Author: Mahrez Amri
Author: Marianna Casavola ORCID iD
Author: Tugce Eralp Erden
Author: Paul Collier
Author: Peter P. Wells ORCID iD

Download statistics

Downloads from ePrints over the past year. Other digital versions may also be available to download e.g. from the publisher's website.

View more statistics

Atom RSS 1.0 RSS 2.0

Contact ePrints Soton: eprints@soton.ac.uk

ePrints Soton supports OAI 2.0 with a base URL of http://eprints.soton.ac.uk/cgi/oai2

This repository has been built using EPrints software, developed at the University of Southampton, but available to everyone to use.

We use cookies to ensure that we give you the best experience on our website. If you continue without changing your settings, we will assume that you are happy to receive cookies on the University of Southampton website.

×