Low temperature atomic layer deposition of PbO2 for electrochemical applications

Bielinski, Ashley R.; Emery, Jonathan D.; Agyapong-Fordjour, Frederick; Jones, Jessica C.; Lopes, Pietro Papa; Martinson, Alex B. F.

doi:10.1088/1361-6528/ad8163

Low temperature atomic layer deposition of PbO₂ for electrochemical applications

Journal Article · Fri Oct 11 04:00:00 EDT 2024 · Nanotechnology

DOI:https://doi.org/10.1088/1361-6528/ad8163· OSTI ID:2997248

^[1]; Emery, Jonathan D. ^[2]; ^[1]; ^[1]; ^[1]; ^[1]

Argonne National Laboratory (ANL), Argonne, IL (United States)
Northwestern Univ., Evanston, IL (United States)

A low temperature atomic layer deposition (ALD) process for PbO₂ was developed using bis(1-dimethylamino-2-methyl-2-propanolate)lead(II), Pb(DMAMP)₂, and O₃ as the reactants, with a high growth rate of 2.6 Å/cycle. PbO₂ readily reduces under low oxygen partial pressures at moderate temperatures making it challenging to deposit ALD PbO₂ from Pb²⁺ precursors. However, thin films deposited with this process showed small crystalline grains of α-PbO₂ and β-PbO₂, without signs of reduced PbO_x phases. The ALD PbO₂ thin films show the high electrical conductivity characteristic of bulk PbO₂. In situ measurements of ALD PbO₂ film conductivity during growth suggest a reaction mechanism by which sub-surface oxygen mobility contributes to the growth of resistive PbO or PbO_x during the Pb(DMAMP)₂ surface reaction step, which is only fully oxidized from Pb²⁺ to Pb⁴⁺ during the O₃ reaction step. These films were electrochemically reduced to PbSO₄ in H₂SO₄ and then reoxidized to PbO₂, demonstrating their suitability for use as an electrode material for fundamental battery research and other electrochemical applications.

View Accepted Manuscript (DOE)

Research Organization:: Argonne National Laboratory (ANL), Argonne, IL (United States)

Sponsoring Organization:: USDOE Office of Science (SC); National Science Foundation (NSF)

Grant/Contract Number:: AC02-06CH11357

OSTI ID:: 2997248

Journal Information:: Nanotechnology, Journal Name: Nanotechnology Journal Issue: 50 Vol. 35; ISSN 1361-6528; ISSN 0957-4484

Publisher:: IOP PublishingCopyright Statement

Country of Publication:: United States

Language:: English

References (28)

Thermal Stability of Lead Oxide Films Prepared by Reactive DC Magnetron Sputtering Venkataraj, S.; Kappertz, O.; Drese, R. physica status solidi (a), Vol. 194, Issue 1 https://doi.org/10.1002/1521-396X(200211)194:1%3C192::AID-PSSA192%3E3.0.CO;2-L	journal	November 2002
The Influence of Ozone: Superstoichiometric Oxygen in Atomic Layer Deposition of Fe ₂ O ₃ Using tert ‐Butylferrocene and O ₃ Schneider, Joel R.; Baker, Jon G.; Bent, Stacey F. Advanced Materials Interfaces, Vol. 7, Issue 11 https://doi.org/10.1002/admi.202000318	journal	April 2020
Atomic Layer Deposition of Co_xO_y Films: Oxidants versus Composition Wan, Zhixin; Zhang, Teng Fei; Zeng, Zhihao Advanced Materials Interfaces, Vol. 9, Issue 14 https://doi.org/10.1002/admi.202200097	journal	April 2022
Preparation of ZnO films with variable electric field-assisted atomic layer deposition technique Lu, Weier; Dong, Yabin; Li, Chaobo Applied Surface Science, Vol. 303 https://doi.org/10.1016/j.apsusc.2014.02.097	journal	June 2014
Anodic electrodeposition of PbO2 on ATO/Ti with simultaneous doping of F, Co, and Fe as super-hydrophilic, highly active, and durable electrocatalyst for oxygen evolution reaction in acidic solution Shamsi, Faezeh; Rezaei, Milad Colloids and Surfaces A: Physicochemical and Engineering Aspects, Vol. 670 https://doi.org/10.1016/j.colsurfa.2023.131608	journal	August 2023
Why is lead dioxide metallic? Payne, David J.; Egdell, Russell G.; Hao, Wang Chemical Physics Letters, Vol. 411, Issue 1-3 https://doi.org/10.1016/j.cplett.2005.06.023	journal	August 2005
EQCM study of hydrated PbO2 content and its influence on cycling performance of lead-acid batteries Wei, Jucai; Gu, Yueyuan; Guo, Zhigang Journal of Energy Storage, Vol. 21 https://doi.org/10.1016/j.est.2019.01.015	journal	February 2019
The importance of the non-stoichiometry of lead dioxide and the location of hydrogen in the positive active mass of the lead–acid battery Moseley, Patrick T.; Steele, Ian M. Journal of Energy Storage, Vol. 61 https://doi.org/10.1016/j.est.2023.106754	journal	May 2023
Exploiting volatile lead compounds as precursors for the atomic layer deposition of lead dioxide thin films Harjuoja, Jenni; Putkonen, Matti; Niinistö, Lauri Thin Solid Films, Vol. 497, Issue 1-2 https://doi.org/10.1016/j.tsf.2005.09.188	journal	February 2006
Understanding and Utilizing Reactive Oxygen Reservoirs in Atomic Layer Deposition of Metal Oxides with Ozone Schneider, Joel R.; de Paula, Camila; Richey, Nathaniel E. Chemistry of Materials, Vol. 34, Issue 12 https://doi.org/10.1021/acs.chemmater.2c00753	journal	June 2022
Oxidation State Discrimination in the Atomic Layer Deposition of Vanadium Oxides Weimer, Matthew S.; Kim, In Soo; Guo, Peijun Chemistry of Materials, Vol. 29, Issue 15 https://doi.org/10.1021/acs.chemmater.7b01130	journal	July 2017
Rapid Growth of Crystalline Mn ₅ O ₈ by Self-Limited Multilayer Deposition using Mn(EtCp) ₂ and O ₃ Young, Matthias J.; Hare, Christopher D.; Cavanagh, Andrew S. ACS Applied Materials & Interfaces, Vol. 8, Issue 28 https://doi.org/10.1021/acsami.6b04529	journal	July 2016
Surface Loss in Ozone-Based Atomic Layer Deposition Processes Knoops, Harm C.M.; Elam, Jeffrey W.; Libera, Joseph A. Chemistry of Materials, Vol. 23, Issue 9, p. 2381-2387 https://doi.org/10.1021/cm2001144	journal	May 2011
Unusual Growth Behavior of Atomic Layer Deposited PbTiO₃ Thin Films Using Water and Ozone As Oxygen Sources and Their Combination Lee, Hyun Ju; Park, Min Hyuk; Min, Yo-Sep The Journal of Physical Chemistry C, Vol. 114, Issue 29 https://doi.org/10.1021/jp101423f	journal	July 2010
Phase Discrimination through Oxidant Selection in Low-Temperature Atomic Layer Deposition of Crystalline Iron Oxides Riha, Shannon C.; Racowski, Joy M.; Lanci, Michael P. Langmuir, Vol. 29, Issue 10 https://doi.org/10.1021/la305027k	journal	February 2013
The other model antiferroelectric: PbHfO ₃ thin films from ALD precursors Hanrahan, Brendan; Milesi-Brault, Cosme; Leff, Asher APL Materials, Vol. 9, Issue 2 https://doi.org/10.1063/5.0035730	journal	February 2021
Evaluating an electric field modulated plasma enhanced atomic layer deposition of platinum layers on different substrates Yan, Mingming; Zhang, Tianchong; Wang, Bo Journal of Applied Physics, Vol. 134, Issue 15 https://doi.org/10.1063/5.0157164	journal	October 2023
Nature of the Band Gap and Origin of the Conductivity of PbO 2 Revealed by Theory and Experiment Scanlon, David O.; Kehoe, Aoife B.; Watson, Graeme W. Physical Review Letters, Vol. 107, Issue 24 https://doi.org/10.1103/PhysRevLett.107.246402	journal	December 2011
Quantitative texture analysis by Rietveld refinement Von Dreele, R. B. Journal of Applied Crystallography, Vol. 30, Issue 4 https://doi.org/10.1107/S0021889897005918	journal	August 1997
Structural Studies of Rutile-Type Metal Dioxides Bolzan, A. A.; Fong, C.; Kennedy, B. J. Acta Crystallographica Section B Structural Science, Vol. 53, Issue 3 https://doi.org/10.1107/S0108768197001468	journal	June 1997
Growth of thin film ferroelectric PZT, PHT, and antiferroelectric PHO from atomic layer deposition precursors Strnad, Nicholas A.; Hanrahan, Brendan M.; Potrepka, Daniel M. Journal of the American Ceramic Society, Vol. 104, Issue 3 https://doi.org/10.1111/jace.17521	journal	November 2020
Texture and phase variation of ALD PbTiO3 films crystallized by rapid thermal anneal Strnad, Nicholas A.; Potrepka, Daniel M.; Pulskamp, Jeffrey S. Journal of Vacuum Science & Technology A: Vacuum, Surfaces, and Films, Vol. 37, Issue 2 https://doi.org/10.1116/1.5080226	journal	February 2019
Comprehensive characterization of copper oxide atomic layer deposition using water or ozone with enhanced bis-(dimethylamino-2-propoxide) copper delivery Avila, Jason R.; Eddy, Charles R.; Wheeler, Virginia D. Journal of Vacuum Science & Technology A, Vol. 38, Issue 4 https://doi.org/10.1116/6.0000248	journal	July 2020
Electrical Properties of Electrodeposited PbO[sub 2] Films Mindt, W. Journal of The Electrochemical Society, Vol. 116, Issue 8 https://doi.org/10.1149/1.2412217	journal	January 1969
Atomic Layer Deposition and Electrical Properties of PbTiO[sub 3] Thin Films Using Metallorganic Precursors and H[sub 2]O Weon Hwang, Gyu; Ju Lee, Hyun; Lee, Keun Journal of The Electrochemical Society, Vol. 154, Issue 3 https://doi.org/10.1149/1.2431317	journal	January 2007
The Electrical Conductivity of Lead Dioxide Thomas, Upton B. Journal of The Electrochemical Society, Vol. 94, Issue 2 https://doi.org/10.1149/1.2773823	journal	January 1948
The Effects of Oxidants on the Growth Behavior of PbTiO3 Thin Film by Atomic Layer Deposition Lee, Hyun Ju; Park, Min Hyuk; Hwang, Cheol Seong ECS Transactions, Vol. 19, Issue 2 https://doi.org/10.1149/1.3122137	journal	May 2009
Thermodynamic description of the Pb-O system Risold, D.; Nagata, J. -I.; Suzuki, R. O. Journal of Phase Equilibria, Vol. 19, Issue 3 https://doi.org/10.1361/105497198770342238	journal	June 1998

Similar Records

Kinetics of oxidation processes on lead electrode in H{sub 2}SO{sub 4}. 2: The growth of the PbSO{sub 4} and PbO layer

Journal Article · Sun Oct 01 00:00:00 EDT 1995 · Journal of the Electrochemical Society · OSTI ID:131771

Electrochemical properties of the basic lead sulfate layers on Pb in H{sub 2}SO{sub 4}

Journal Article · Tue Nov 30 23:00:00 EST 1993 · Journal of the Electrochemical Society · OSTI ID:142173

ELECTROCHEMICAL PROPERTIES OF PbO$sub 2$ AND THE ANODIC CORROSION OF LEAD AND LEAD ALLOYS

Journal Article · Tue Jul 01 00:00:00 EDT 1958 · Journal of the Electrochemical Society (U.S.) Absorbed Electrochem. Technol. · OSTI ID:4313479

Related Subjects

atomic layer deposition
in situ conductivity
lead acid batteries
lead dioxide

Low temperature atomic layer deposition of PbO2 for electrochemical applications

Citation Formats

References (28)

Similar Records

Related Subjects

Low temperature atomic layer deposition of PbO₂ for electrochemical applications