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4. The synthesis and characterisation of single-walled carbon nanotubes and graphene for electrochemical applications

Author

Miller, Thomas S.

Subjects
540, QD Chemistry
Abstract

In recent years sp2 carbon materials, including single-walled carbon nanotubes (SWNT) and graphene have attracted significant attention, especially in the field of electrochemistry. However there is a marked disparity of opinion concerning the fundamental inherent electron transfer (ET) properties of these materials, largely due to complications regarding their synthesis, characterisation and the methods utilised to measure their electrochemical characteristics. As shown in this thesis, catalysed chemical vapour deposition (cCVD) allows the growth of very high quality SWNT directly onto insulating substrates and so it is considered by many to be the ideal method to produce SWNT for fundamental studies and applications. However, graphene must be transferred post cCVD growth to insulating substrates, as it grows on metal foil catalysts and this process is currently associated with issues with contamination and mechanical damage. In this thesis SWNTs with both 2D and 3D geometries are investigated using micro- or nano- scale capillary electrochemical methods. By using outer sphere redox mediators and by isolating the SWNT sidewalls and end-caps it is shown that ET at SWNTs is both fast and occurs on both pristine sidewalls and closed ends. This opposes the commonly held view that ET only happens at open ends and defects. Then, it is shown that functionality can be introduced into pristine SWNTs either by platinum nanoparticle (NP) electrodeposition or anodic pre-treatment. These activated SWNTs are shown to display improved ET to a range of complex and inner sphere redox reactions, including becoming electrocatalytic for the oxygen reduction reaction (ORR) and the methanol oxidation reaction (MOR). Also in this thesis a method of performing generation/collection (G/C) electrochemical measurements within the meniscus of a microcapillary is demonstrated. This system is shown to be effective at both investigating processes on complex electrode surfaces and at investigating the mechanistic aspects of the ORR.

Published
2013

5. Production of phosphorene nanoribbons

Author

Watts, Mitchell C., Picco, Loren, Russell-Pavier, Freddie S., Cullen, Patrick L., Miller, Thomas S., Bartuś, Szymon P., Payton, Oliver D., Skipper, Neal T., Tileli, Vasiliki, and Howard, Christopher A.

Published
2019
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7. Ultrasmall, Coating-Free, Pyramidal Platinum Nanoparticles for High Stability Fuel Cell Oxygen Reduction

Author

Universidad de Alicante. Departamento de Química Física, Universidad de Alicante. Instituto Universitario de Electroquímica, Mastronardi, Valentina, Magliocca, Emanuele, Solla-Gullón, José, Brescia, Rosaria, Pompa, Pier Paolo, Miller, Thomas S., Moglianetti, Mauro, Universidad de Alicante. Departamento de Química Física, Universidad de Alicante. Instituto Universitario de Electroquímica, Mastronardi, Valentina, Magliocca, Emanuele, Solla-Gullón, José, Brescia, Rosaria, Pompa, Pier Paolo, Miller, Thomas S., and Moglianetti, Mauro

Abstract

Ultrasmall (<5 nm diameter) noble metal nanoparticles with a high fraction of {111} surface domains are of fundamental and practical interest as electrocatalysts, especially in fuel cells; the nanomaterial surface structure dictates its catalytic properties, including kinetics and stability. However, the synthesis of size-controlled, pure Pt-shaped nanocatalysts has remained a formidable chemical challenge. There is an urgent need for an industrially scalable method for their production. Here, a one-step approach is presented for the preparation of single-crystal pyramidal nanocatalysts with a high fraction of {111} surface domains and a diameter below 4 nm. This is achieved by harnessing the shape-directing effect of citrate molecules, together with the strict control of oxidative etching while avoiding polymers, surfactants, and organic solvents. These catalysts exhibit significantly enhanced durability while, providing equivalent current and power densities to highly optimized commercial Pt/C catalysts at the beginning of life (BOL). This is even the case when they are tested in full polymer electrolyte membrane fuel cells (PEMFCs), as opposed to rotating disk experiments that artificially enhance electrode kinetics and minimize degradation. This demonstrates that the {111} surface domains in pyramidal Pt nanoparticles (as opposed to spherical Pt nanoparticles) can improve aggregation/corrosion resistance in realistic fuel cell conditions, leading to a significant improvement in membrane electrode assembly (MEA) stability and lifetime.

Published
2022

8. Neutron studies of Na-ion battery materials

Author

Shah, Ami R, primary, Shutt, Rebecca R C, additional, Smith, Keenan, additional, Hack, Jennifer, additional, Neville, Tobias P, additional, Headen, Thomas F, additional, Brett, Dan J L, additional, Howard, Christopher A, additional, Miller, Thomas S, additional, and Cullen, Patrick L, additional

Published
2021
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10. 2021 roadmap on lithium sulfur batteries

Author

Robinson, James B, primary, Xi, Kai, additional, Kumar, R Vasant, additional, Ferrari, Andrea C, additional, Au, Heather, additional, Titirici, Maria-Magdalena, additional, Parra-Puerto, Andres, additional, Kucernak, Anthony, additional, Fitch, Samuel D S, additional, Garcia-Araez, Nuria, additional, Brown, Zachary L, additional, Pasta, Mauro, additional, Furness, Liam, additional, Kibler, Alexander J, additional, Walsh, Darren A, additional, Johnson, Lee R, additional, Holc, Conrad, additional, Newton, Graham N, additional, Champness, Neil R, additional, Markoulidis, Foivos, additional, Crean, Carol, additional, Slade, Robert C T, additional, Andritsos, Eleftherios I, additional, Cai, Qiong, additional, Babar, Shumaila, additional, Zhang, Teng, additional, Lekakou, Constantina, additional, Kulkarni, Nivedita, additional, Rettie, Alexander J E, additional, Jervis, Rhodri, additional, Cornish, Michael, additional, Marinescu, Monica, additional, Offer, Gregory, additional, Li, Zhuangnan, additional, Bird, Liam, additional, Grey, Clare P, additional, Chhowalla, Manish, additional, Lecce, Daniele Di, additional, Owen, Rhodri E, additional, Miller, Thomas S, additional, Brett, Dan J L, additional, Liatard, Sebastien, additional, Ainsworth, David, additional, and Shearing, Paul R, additional

Published
2021
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11. Aquaporin-like water transport in nanoporous crystalline layered carbon nitride

Author

Foglia, Fabrizia, primary, Clancy, Adam J., additional, Berry-Gair, Jasper, additional, Lisowska, Karolina, additional, Wilding, Martin C., additional, Suter, Theo M., additional, Miller, Thomas S., additional, Smith, Keenan, additional, Demmel, Franz, additional, Appel, Markus, additional, Sakai, Victoria García, additional, Sella, Andrea, additional, Howard, Christopher A., additional, Tyagi, Madhusudan, additional, Corà, Furio, additional, and McMillan, Paul F., additional

Published
2020
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12. Synthesis, Structure and Electronic Properties of Graphitic Carbon Nitride Films

Author

Suter, Theo, Brázdová, Veronika, McColl, Kit, Miller, Thomas S., Nagashima, Hiroki, Salvadori, Enrico, Sella, Andrea, Howard, Christopher A., Kay, Christopher W. M., Corà, Furio, and McMillan, Paul F.

Subjects
Surfaces, Coatings and Films, Energy (all), Electronic, Optical and Magnetic Materials, Physical and Theoretical Chemistry, Electronic, Optical and Magnetic Materials, Surfaces, Coatings and Films
Published
2019
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15. Carbon Nitride Materials as Efficient Catalyst Supports for Proton Exchange Membrane Water Electrolyzers.

Author

Jorge, Ana Belen, Dedigama, Ishanka, Miller, Thomas S., Shearing, Paul, Brett, Daniel J. L., and McMillan, Paul F.

Subjects
PROTON exchange membrane fuel cells, ELECTROCATALYSTS, ELECTROLYTIC cells
Abstract

Carbon nitride materials with graphitic to polymeric structures (gCNH) were investigated as catalyst supports for the proton exchange membrane (PEM) water electrolyzers using IrO2 nanoparticles as oxygen evolution electrocatalyst. Here, the performance of IrO2 nanoparticles formed and deposited in situ onto carbon nitride support for PEM water electrolysis was explored based on previous preliminary studies conducted in related systems. The results revealed that this preparation route catalyzed the decomposition of the carbon nitride to form a material with much lower N content. This resulted in a significant enhancement of the performance of the gCNH-IrO2 (or N-doped C-IrO2) electrocatalyst that was likely attributed to higher electrical conductivity of the N-doped carbon support. [ABSTRACT FROM AUTHOR]

Published
2018
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16. 2021 roadmap on lithium sulfur batteries

Author

Constantina Lekakou, R. Vasant Kumar, Conrad Holc, Nuria Garcia-Araez, Thomas S. Miller, Nivedita Kulkarni, Alexander J. E. Rettie, Clare P. Grey, Manish Chhowalla, David Ainsworth, Shumaila Babar, Maria-Magdalena Titirici, Mauro Pasta, Liam Bird, Neil R. Champness, Michael Cornish, Darren A. Walsh, Andrea C. Ferrari, Carol Crean, Gregory J. Offer, Paul R. Shearing, Foivos Markoulidis, Samuel D. S. Fitch, James B. Robinson, Daniele Di Lecce, Lee Johnson, Alexander J. Kibler, Rhodri E. Owen, Heather Au, Eleftherios I. Andritsos, Zhuangnan Li, Kai Xi, Dan J. L. Brett, Liam Furness, Zachary L. Brown, Anthony Kucernak, Graham N. Newton, Monica Marinescu, Teng Zhang, Sebastien Liatard, Qiong Cai, Robert C. T. Slade, Andres Parra-Puerto, Rhodri Jervis, Robinson, James B [0000-0002-6509-7769], Xi, Kai [0000-0003-0508-7910], Ferrari, Andrea C [0000-0003-0907-9993], Au, Heather [0000-0002-1652-2204], Titirici, Maria-Magdalena [0000-0003-0773-2100], Parra-Puerto, Andres [0000-0002-1131-1168], Kucernak, Anthony [0000-0002-5790-9683], Fitch, Samuel D S [0000-0002-3681-8985], Garcia-Araez, Nuria [0000-0001-9095-2379], Brown, Zachary L [0000-0003-0772-3159], Pasta, Mauro [0000-0002-2613-4555], Furness, Liam [0000-0003-3538-2929], Kibler, Alexander J [0000-0002-4441-4294], Walsh, Darren A [0000-0003-3691-6734], Johnson, Lee R [0000-0002-1789-814X], Holc, Conrad [0000-0003-4412-3443], Newton, Graham N [0000-0003-2246-4466], Champness, Neil R [0000-0003-2970-1487], Markoulidis, Foivos [0000-0002-3811-0104], Crean, Carol [0000-0003-0756-7504], Slade, Robert C T [0000-0002-5449-5702], Andritsos, Eleftherios I [0000-0002-3289-266X], Cai, Qiong [0000-0002-1677-0515], Zhang, Teng [0000-0002-3657-5151], Lekakou, Constantina [0000-0003-4494-1761], Kulkarni, Nivedita [0000-0002-3115-629X], Rettie, Alexander J E [0000-0002-2482-9732], Jervis, Rhodri [0000-0003-2784-7802], Marinescu, Monica [0000-0003-1641-3371], Offer, Gregory [0000-0003-1324-8366], Li, Zhuangnan [0000-0001-8154-1287], Grey, Clare P [0000-0001-5572-192X], Chhowalla, Manish [0000-0002-8183-4044], Lecce, Daniele Di [0000-0003-1290-1140], Owen, Rhodri E [0000-0002-1246-2988], Miller, Thomas S [0000-0002-2224-5768], Brett, Dan J L [0000-0002-8545-3126], Shearing, Paul R [0000-0002-1387-9531], Apollo - University of Cambridge Repository, Robinson, JB [0000-0002-6509-7769], Xi, K [0000-0003-0508-7910], Ferrari, AC [0000-0003-0907-9993], Au, H [0000-0002-1652-2204], Titirici, MM [0000-0003-0773-2100], Puerto, AP [0000-0002-1131-1168], Kucernak, A [0000-0002-5790-9683], Fitch, SDS [0000-0002-3681-8985], Araez, NG [0000-0001-9095-2379], Brown, ZL [0000-0003-0772-3159], Pasta, M [0000-0002-2613-4555], Furness, L [0000-0003-3538-2929], Kibler, AJ [0000-0002-4441-4294], Walsh, DA [0000-0003-3691-6734], Johnson, LR [0000-0002-1789-814X], Holc, C [0000-0003-4412-3443], Newton, GN [0000-0003-2246-4466], Champness, NR [0000-0003-2970-1487], Markoulidis, F [0000-0002-3811-0104], Crean, C [0000-0003-0756-7504], Slade, RCT [0000-0002-5449-5702], Andritsos, EI [0000-0002-3289-266X], Cai, Q [0000-0002-1677-0515], Zhang, T [0000-0002-3657-5151], Lekakou, C [0000-0003-4494-1761], Kulkarni, N [0000-0002-3115-629X], Rettie, AJE [0000-0002-2482-9732], Jervis, R [0000-0003-2784-7802], Marinescu, M [0000-0003-1641-3371], Offer, G [0000-0003-1324-8366], Li, Z [0000-0001-8154-1287], Grey, CP [0000-0001-5572-192X], Chhowalla, M [0000-0002-8183-4044], Lecce, DD [0000-0003-1290-1140], Owen, RE [0000-0002-1246-2988], Miller, TS [0000-0002-2224-5768], Brett, DJL [0000-0002-8545-3126], Shearing, PR [0000-0002-1387-9531], Kumar, Ramachandran [0000-0001-9223-2332], Ferrari, Andrea [0000-0003-0907-9993], and Grey, Clare [0000-0001-5572-192X]

Subjects
polysulfide shuttle, Technology, Energy & Fuels, Materials Science (miscellaneous), Materials Science, Materials Science, Multidisciplinary, 02 engineering and technology, 010402 general chemistry, lithium sulfur batteries, 7. Clean energy, 01 natural sciences, battery modelling, Research community, Materials Chemistry, Lithium sulfur, Government, Science & Technology, carbon materials, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Economies of scale, Engineering management, General Energy, Roadmap, Li-metal anode, Energy density, 0210 nano-technology, Electrochemical energy storage
Abstract

Batteries that extend performance beyond the intrinsic limits of Li-ion batteries are among the most important developments required to continue the revolution promised by electrochemical devices. Of these next-generation batteries, lithium sulfur (Li–S) chemistry is among the most commercially mature, with cells offering a substantial increase in gravimetric energy density, reduced costs and improved safety prospects. However, there remain outstanding issues to advance the commercial prospects of the technology and benefit from the economies of scale felt by Li-ion cells, including improving both the rate performance and longevity of cells. To address these challenges, the Faraday Institution, the UK’s independent institute for electrochemical energy storage science and technology, launched the Lithium Sulfur Technology Accelerator (LiSTAR) programme in October 2019. This Roadmap, authored by researchers and partners of the LiSTAR programme, is intended to highlight the outstanding issues that must be addressed and provide an insight into the pathways towards solving them adopted by the LiSTAR consortium. In compiling this Roadmap we hope to aid the development of the wider Li–S research community, providing a guide for academia, industry, government and funding agencies in this important and rapidly developing research space.

Published
2021

17. Formation of an ion-free crystalline carbon nitride and its reversible intercalation with ionic species and molecular water.

Author

Suter TM, Miller TS, Cockcroft JK, Aliev AE, Wilding MC, Sella A, Corà F, Howard CA, and McMillan PF

Abstract

The development of processes to tune the properties of materials is essential for the progression of next-generation technologies for catalysis, optoelectronics and sustainability including energy harvesting and conversion. Layered carbon nitrides have also been identified as of significant interest within these fields of application. However, most carbon nitride materials studied to date have poor crystallinity and therefore their properties cannot be readily controlled or easily related to their molecular level or nanoscale structures. Here we report a process for forming a range of crystalline layered carbon nitrides with polytriazine imide (PTI) structures that can be interconverted by simple ion exchange processes, permitting the tunability of their optoelectronic and chemical properties. Notable outcomes of our work are (a) the creation of a crystalline, guest-ion-free PTI compound that (b) can be re-intercalated with ions or molecules using "soft chemistry" approaches. This includes the intercalation of HCl, demonstrating a new ambient pressure route to the layered PTI· x HCl material that was previously only available by a high-pressure-high-temperature route (c). Our work also shows (d) that the intercalant-free (IF-) PTI material spontaneously absorbs up to 10 weight% H 2 O from the ambient atmosphere and that this process is reversible, leading to potential applications for membranes and water capture in dry environments.

Published
2018
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