Crystalline Thin Films: The Electrochemical Atomic Layer Deposition (ECALD) view. MMALEWANE MODIBEDI

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1 Crystalline Thin Films: The Electrochemical Atomic Layer Deposition (ECALD) view MMALEWANE MODIBEDI

2 Acknowledgements Outline Context: Crystalline Thin films What is ECALD? Mechanism Instrumental set-up Applications - Electrocatalysis Deposition on various substrates: work EaP - Compound semiconductor Conclusions CSIR

3 Acknowledgements Dr. Tumaini Mkwizu, PhD work on ECALD Ms. Nikiwe Kunjuzwa, PhD student- ECALD and batteries Prof. Kenneth Ozoemena, Research group leader and electrochemist Dr Mkhulu Mathe, Competence area manager, electrochemist and ECALD expert

4 Crystalline Thin Films Application Historical: light absorber material CdTe, crystalline Si Modern: light absorber material Solar cells Cu, In, Ga, Se (CIGS)- developed by Vivian Alberts and UJ - low material cost in potentially low fabrication costs Growth methodologies Molecular beam epitaxy/ chemical vapour deposition Disadvantages: expensive equipment, use toxic precursors, Vacuum and High Temperature Electrochemical methods: co-deposition, precipitation Disadvantages: lack of control during deposition

5 What is ECALD? Definition: alternated electrodeposition of atomic layers of elements on a substrate, employing under-potential deposition (UPD) in which one element deposits onto another element at a voltage prior to that necessary to deposit the element onto itself. Advantages: ambient temperature, use small concentrations of precursor solutions, optimized solutions and potential separately Offers atomic layer control- fundamental for controlled growth processes

6 M1-BE Rinse M1-Fill M1-Deposit M2-BE Rinse M2-Fill M2-Deposit M1-BE Rinse M1-Fill M1-Deposit M2-BE Rinse M2-Fill M2-Deposit Steps Mechanism-Sequential deposition Cycle 1 Cycle 2 Repeat Cycles Time

7 Distribution Valve Block Waste/ Recycling Reference Electrode Electrodeposition flow-cell Pump Counter Electrode Pump Pump Substrate (Working Electrode) Gasket Pump Potentiostat Pump Computer Interface/ DAQ Card Relay Board/ Power Supply Precursor Solution Reservoirs

8 Potentiostat Flow-cell Peristaltic Pumps Instrumental set-up Pumping system, Potentiostat and Flow-Cell Connectivity

9 APPLICATIONS Electrocatalysis Noble-Metals studied = Pt, Ru, Au, Pd Substrates = Carbon materials-fuel cell carbon paper, Gold films T.S.Mkwizu, M.K. Mathe, and I. Cukrowski, ECS Transactions, Vol.19, (2009) T.S.Mkwizu, M.K. Mathe, and I. Cukrowski, Langmuir, Vol. 26, (2010) T.S Mkwizu, M.R. Modibedi, and M. K. Mathe, 219 th ECS Meeting (2011)

10 Sequential electrodeposition coupled to Surface-limited Redoxreplacement reactions: Synthesis of multilayered bimetallic RuPt electrocatalyst S S S S S S S (1) Clean substrate with blank electrolyte (BE); Inject Cu 2+ solution at E >> E Cu-Cu2+ S S S S S S S Pt Pt Pt Pt Pt S S S S S S S Cu Cu Cu Cu Cu Cu 2+ -2e Cu 2+ Cu2+ S S S S S S S Pt Cu Pt Cu Cu (2) Potentiostatic electrodeposition at E dep > E Cu-Cu2+ (Underpotential Deposition (UPD)) or E dep < E Cu-Cu2+ (small Overpotential Deposition (OPD) - to produce sacrificial Cu adlayer on active sites of the substrate; Rinse with BE (4) Pt nanodeposit on substrate; Rinse with BE and inject Cu 2+ solution at E >> E Cu-Cu2+ Pt 4+ Cu 2+ Pt 4+ (3) Inject H 2 PtCl 6 solution and allow surface-limited redox-replacement (SLRR) of Cu by Pt at open circuit (OC) S S S S S S S Pt Pt Pt Pt Pt Cu Cu Cu Cu Cu Cu 2+ -2e Cu2+ Cu 2+ (5) Potentiostatic electrodeposition at E dep to produce sacrificial Cu adlayer on active sites on Pt adlayers; Rinse with BE S S S S S S S Pt Pt Pt Pt Pt Ru Cu Ru Ru Cu Ru 3+ Ru 3+ Cu 2+ (6) Inject RuCl 3 solution and allow surface-limited redox-replacement (SLRR) of Cu by Ru at OC S S S S S S S Pt Pt Pt Pt Pt Ru Ru Ru Ru Ru S S S S S S S Pt Pt Pt Pt Pt Ru Ru Ru Ru Ru Pt Pt Pt Pt Pt Ru Ru Ru Ru Ru

11 Tuning Electrocatalysis: Electrochemical Characterisation Electro-activity increases with increasing deposition cycles Impedance of methanol electro-oxidation Pt < PtAu < PtRu Order of activity: Methanol electro-oxidation Chronoamperometry of methanol electro-oxidation T.S.Mkwizu, M.K. Mathe, and I. Cukrowski, ECS Transactions, Vol.19, (2009) T.S.Mkwizu, M.K. Mathe, and I. Cukrowski, Langmuir, Vol. 26, (2010) (i) Sequentially-deposited with Cu SLRR bimetallic PtRu / GC (ii) Sequentially- codeposited with Cu SLRR bimetallic Pt-Ru/GC (iii) Sequentially-deposited with Cu SLRR monometallic Pt/GC 0.1M HClO M CH 3 OH

12 Tuning Electrocatalysis on Fuel Cell gas diffusion layer: SEM micrographs and EDX profile Carbon paper TGPH090 Pt/carbon paper TGPH090 C Carbon paper TGPH090 Pt/carbon paper TGPH090 Pt/carbon paper TGPH090 O Pt Cu Pt Energy (kev)

13 Current Density (ma/cm 2 ) Current Density (ma/cm 2 ) Tuning Electrocatalysis on Fuel Cell gas diffusion layer: Electrochemical Characterisation Methanol oxidation Potential (V) CO adsorption-oxidation 1.0 (ii) 0.1 M HClO4 + CO Cyclic voltammograms at 50 mv/s in (i) 0.1 M HClO M Methanol Pt/carbon paper TGPH090 Carbon paper TGPH Potential (V)

14 Compound Semiconductors Group II - VI, Group III - V, Group IV - VI: Optoelectronic materials CdTe, CdSe, GaAs, HgSe - photovoltaics, photon sensors, lasers etc. Substrates = Gold, carbon material Mkhulu K. Mathe et al. J. Electrochem. Soc., Volume 152, Issue 11, C751-C755 (2005) Mkhulu K. Mathe et al. J. Crystal Growth Volume 271, Issues 1-2, (2004) Energy storage Physical form (capacitors) and Electrochemical form (batteries) Obstacle to increasing thin film battery storage capacity: limited diffusion path length of ions and electrons Solution: area enhancement- 3D thin films - Increases total amount of active material while maintaining short diffusion path - Results- high power and energy density

15 Conclusions ECALD: controlled growth of thin film deposits atomic layer control is key to reducing the amount of PEMFC catalysts possibility of a 3D battery stack

16 Thank You

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