Platinum ALD from Pt(acac)2 and O3: Growth mechanism and electrocatalytic applications
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1 Platinum ALD from Pt(acac)2 and O3: Growth mechanism and electrocatalytic applications Johannes Schumacher, Loïc Assaud, Alexander Tafel, Julien Bachmann Department of Chemistry and Pharmacy, Friedrich-Alexander-Universität Erlangen-Nürnberg
2 Energy conversion: Reactions at surfaces Nanostructures: Control of specific surface area and diffusion paths
3 Energy conversion: Electrons and holes across interfaces Nanostructures: Control of specific surface area and diffusion paths
4 Preparative strategy Towards elongated nanostructures with tunable geometry
5 Platinum Metallic Pt: Electrocatalyst for H2 production from water and for ethanol oxidation (electrolysis, fuel cell) Standard ALD reaction: MeCpPtMe3 + O C Aaltonen, Ritala, Sajavaara, Keinonen, Leskelä, Chem. Mater. 2003, 15, Aaltonen, Ritala, Tung, Chi, Arstila, Meinander, Leskelä, J. Mater. Res. 2004, 19, Costs of Pt ALD precursors (Strem): MeCpPtMe3: 231 / 0.5 g Pt(acac)2: 115 / 1 g Conceivable alternative: Pt(acac)2 + O3 130 C, 140 C Hämäläinen, Munnik, Ritala, Leskelä, Chem. Mater. 2008, 20,
6 A. Reaction mechanism investigation of Pt(acac)2 + O3 Arradiance GEMSTAR reactor, chamber at C Piezoelectric microbalance SQL-310 from Inficon GaPO4 piezoelectric crystal (Inficon R-20) O3 from BMT 803N generator 80 C, several 'boosted' pulses Pt(acac)2 dosage set by the number of pulses
7 A. Reaction mechanism investigation of Pt(acac)2 + O3 Arradiance GEMSTAR reactor, chamber at C Growth rates at 150 C: Piezoelectric microbalance SQL-310 from Inficon GaPO4 piezoelectric crystal (Inficon R-20) O3 from BMT 803N generator 80 C, several 'boosted' pulses Pt(acac)2 dosage set by the number of pulses Long reaction durations: not self-limiting Short reaction times: self-limiting
8 A. Reaction mechanism investigation of Pt(acac)2 + O3 Comparison btw. short and long Pt(acac)2 exposure durations: Mass increase at O3 step: Oxidation of metallic Pt Large mass oscillations at long expo times: 'Deep' oxidation/reduction
9 A. Reaction mechanism investigation of Pt(acac)2 + O3 Al2O3 ALD performed before start of Pt ALD Nucleation (150 C, 4 Pt(acac)2 pulses per cycle, 5 s exposure):
10 A. Reaction mechanism investigation of Pt(acac)2 + O3 Growth at 130 C (self-limited, 0.6 Å(cycle):
11 A. Reaction mechanism investigation of Pt(acac)2 + O3 Growth at 130 C (self-limited, 0.6 Å(cycle):
12 A. Reaction mechanism investigation of Pt(acac)2 + O3 Metastable Pt oxide is a resting state during the ALD cycle Ozone oxidizes the metal in depth Autocatalytic decomposition of oxide triggered by Pt(acac) 2 Literature precedents: Ru ALD and Pt UHV studies Saliba, Tsai, Panja, Koel, Surf. Sci. 1999, 419, Methaapanon, Geyer, Lee, Bent, J. Mater. Chem. 2012, 22,
13 B. Application to porous substrates In self-limited conditions at 130 C
14 B. Application to porous substrates In self-limited conditions at 130 C
15 B. Application to porous substrates Elemental and structural analyses on anodic TiO2 tubes
16 B. Application to porous substrates Ti felts as 'real-world' substrates for electrocatalysts
17 B. Application to porous substrates Ti felts as 'real-world' substrates for electrocatalysts
18 C. Electrocatalysis at nanoporous Pt / TiO2 surfaces Planar anodized sample:
19 C. Electrocatalysis at nanoporous Pt / TiO2 surfaces
20 C. Electrocatalysis at nanoporous Pt / TiO2 surfaces
21 C. Electrocatalysis at nanoporous Pt / TiO2 surfaces H2SO4/H2O on felts:
22 C. Electrocatalysis at nanoporous Pt / TiO2 surfaces
23 C. Electrocatalysis at nanoporous Pt / TiO2 surfaces
24 C. Electrocatalysis at nanoporous Pt / TiO2 surfaces
25 C. Electrocatalysis at nanoporous Pt / TiO2 surfaces
26 Conclusions Surface chemistry of Pt(acac)2 at oxidized Pt surface can be selflimiting at C dosage is crucial Optimization of electrocatalytic performance by nanostructuring
27 Conclusions Surface chemistry of Pt(acac)2 at oxidized Pt surface can be selflimiting at C dosage is crucial Optimization of electrocatalytic performance by nanostructuring Similar results obtained with galvanically deposited Pt Roscher, Licklederer, Schumacher, Reyes Rios, Hoffmann, Christiansen, Bachmann, Dalton Trans. 2014, 43,
28 Acknowledgements BMBF (project TubulAir±) Johannes Schumacher Dr. Loïc Assaud Alexander Tafel XRD: S. Bochmann (FAU inorganic chemistry), Prof. W. Peukert (FAU materials science) FE-SEM: Dr. S. Christiansen (MPI for the Science of Light, Erlangen)
29
30 Electrodeposited, structured Pt electrode surfaces Nanotubular Pt surface: electrochemically active in acidic and ethanolic solution
31 Transport effects at structured electrode surfaces Steady-state electrolytic currents at Pt, various lengths L: Hexacyanoferrate oxidation: fast reaction, diffusion-limited Proton reduction: slow reaction, surface-limited Ethanol oxidation: slow reaction, surface-limited
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