Tailoring in-situ growth of nanoparticles towards applications
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1 The Hydrogen & Fuel Cell Researcher Conference Tailoring in-situ growth of nanoparticles towards applications Dragos Neagu and John TS Irvine 16 th - 18 th December 2013, University of Birmingham
2 Introduction & Motivation Surfaces decorated with uniformly dispersed catalytically active nanoparticles play a key role in many fields including renewable energy and catalysis. Deposition techniques (e.g. infiltration) In-situ growth of nanoparticles from perovskites (exsolution) Oxidising conditions Reducing conditions
3 Background Previous work on exsolution from perovskites (ABO 3 ): M x O y + y 2 H 2 Reduction xm 0 900C +yh 2 O G red. Only A/B stoichiometric perovskites Both A and B-site containing species upon exsolution Cation reducibility single driving force (only easy to reduce cations were exsolved) Exsolution occurs predominantly in the bulk rather than on the surface This study Most known exsolutions Y. Nishihata, J. Mizuki, T. Akao, H. Tanaka, M. Uenishi, M. Kimura, T. Okamoto, and N. Hamada, Nature, 2002, 418, H. Tanaka, M. Uenishi, M. Taniguchi, I. Tan, K. Narita, M. Kimura, K. Kaneko, Y. Nishihata, and J. Mizuki, Catal. Today, 2006, 117, B. D. Madsen, W. Kobsiriphat, Y. Wang, L. D. Marks, and S. Barnett, ECS Trans., 2007, vol. 7, pp M. B. Katz, S. Zhang, Y. Duan, H. Wang, M. Fang, K. Zhang, B. Li, G. W. Graham, and X. Pan, J. Catal., 2012, 293,
4 Defects in perovskites: how and why? The ideal perovskite structure (ABO3) The role of A-site vacancies in the exsolution of the B-site species H2 B Perovskite nonstoichiometry (A1±αBO3±γ) O A VA Perovskite nonstoichiometry and B-site exsolution
![86 ] Perovskite surface ( extended defect?](/docs-images/91/106746858/images/5-6.jpg ") Surface structuring α = 0.")
5 Cleaving Co 0 exsolutions Key factors controlling particle exsolution Ni 0 exsolutions (Ageing, 900C, ~3%H 2 O/5%H 2 /Ar, 60h) TiO 2-δ exsolutions NO Ni Ni 0 exsolutions 0 from from A 0.8 ABO 3+γ α = 0.2 [La Sr Sr Ni Ni Ti Ti OO 3+γ 3 ] Intrinsic factors Defects A-site vacancies (A 1-α BO 3 ) B-site dopants (A 1-α M x B 1-x O 3 ) O vacancies (A 1-α BO 3-γ ) α = 0.1 Native surface [A 1.3 BO 3.86 ] Perovskite surface ( extended defect?) Surface structuring α = 0.05 Ni 0 exsolutions from A 0.8 BO 3 [La 0.52 Sr 0.28 Ni 0.06 Ti 0.94 O 3 ] [A 0.8 BO 3 ] Extrinsic factors po 2 Atmosphere composition Temperature α = 0 [A 1.3 BO 3.86 ]
6 Example of tailored nonstoichiometry for native surface particle coverage La 0.8 Ce 0.1 Ni 0.4 Ti 0.6 O 3 Ni particles
7 Intensity (au) Alloy nanoparticles A 1-α M x M y B 1-x-y O 3 M 0 + M 0 MM alloy? La 0.5 Sr 0.4 Fe 0.1 Ni 0.1 Ti 0.8 O Fe Co Ni Energy (kev)
8 Interfaces Motivation - e.g. for metal supported solid oxide fuel cells (The METSAPP Project) The need to attach a redox stable perovskite anode layer onto porous steel supports Perovskites anchored onto Metals through metallic exsolutions La 0.49 Sr 0.31 Fe 0.03 Ni 0.03 Ti 0.94 O 3 Metal Anode Perovskite Perovskite Porous metal support Metal Metal Metal Perovskite Generation Composition Impreg. Thicknesse Base case (G1) MS: G1 AFL: FeCr + ScYSZ (60/40) E: ScYSZ Ni-CGO MS: 300 µ AFL: 30 µm E: 16 µm
![High temperature steam electrolysis Work by Dr. George Tsekouras A 1-α BO 3-γ [La 0.4 Sr 0.4 M 0.06 Ti 0.94 O 3-γ ] ABO 3+γ [La 0.3 Sr 0.7 M 0.06 Ti 0.94 O 3+γ ] Carrier gas and steam: 47% H 2 O / 53% N 2 at 900 C Conditioning: - 1.](/docs-images/91/106746858/images/9-0.jpg "7 V for 2-5 min; Scan rate: 10 mv s -1 YSZ (2 mm) Anode (Air) LSM (~ 5 μm) LSM/YSZ (~5 μm) Perovskite cathode (~10 μm) Cathode (Steam/N 2 )")
9 High temperature steam electrolysis Work by Dr. George Tsekouras A 1-α BO 3-γ [La 0.4 Sr 0.4 M 0.06 Ti 0.94 O 3-γ ] ABO 3+γ [La 0.3 Sr 0.7 M 0.06 Ti 0.94 O 3+γ ] Carrier gas and steam: 47% H 2 O / 53% N 2 at 900 C Conditioning: V for 2-5 min; Scan rate: 10 mv s -1 YSZ (2 mm) Anode (Air) LSM (~ 5 μm) LSM/YSZ (~5 μm) Perovskite cathode (~10 μm) Cathode (Steam/N 2 )
10 More on our exsolution work My 1. Neagu, D., Tsekouras, G., Miller, D. N., Ménard, H. & Irvine, J. T. S. In situ growth of nanoparticles through control of non-stoichiometry. Nat. Chem. 5, (2013). 2. Tsekouras, G., Neagu, D. & Irvine, J. T. S. Step-change in high temperature steam electrolysis performance of perovskite oxide cathodes with exsolution of B-site dopants. Energy Environ. Sci. 6, (2012). 3. Gamble, S., Neagu, D. & Irvine, J. T. S. Calculation of a Standard Reformed Biogas Composition and Testing on SOFC Anode Powders. ECS Trans. 57, (2013). 4. Neagu, D. & Irvine, J. T. S. in Compr. Inorg. Chem. II Second Ed. (Editors-in- Chief: Jan Reedijk & Kenneth Poeppelmeier) (Elsevier, 2013). Poster Syed Bukhari, on Cu exsolutions
11 Acknowledgments Collaborators Dr. George Tsekouras (formerly at St Andrews, currently at EMPA, Electrolysis) Dr. David N. Miller (St Andrews, TEM) Dr. Hervé Ménard & SASOL (SASOL St Andrews, XPS) Dr. Paul Connor (St Andrews, Experimental setups) Dr. Peter Blennow (currently at TOPSOE Fuel Cells) & the Risoe DTU team involved in the METSAPP project (steel supports and powders) Funding Supergen XIV Project Delivery of Sustainable Hydrogen European Project METSAPP Thank you for your attention!
In situ growth of nanoparticles through control of non-stoichiometry
DOI: 10.1038/NCHEM.1773 In situ growth of nanoparticles through control of non-stoichiometry Dragos Neagu 1 *, George Tsekouras 1, David N. Miller 1, Hervé Ménard 2 and John T.S. Irvine 1 * 1 University
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