Electrothermal Annealing of Catalytic Platinum Microwire Electrodes: Towards Membrane‐Free pH 7 Glucose Micro‐Fuel Cells

Weber, Jan; Wain, Andrew J.; Attard, Gary Anthony; Marken, Frank

doi:10.1002/elan.201600443

Cited by 6 publications

(5 citation statements)

References 27 publications

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“…The oxidation of glucose on platinum is known to be very sensitive to poisons such as chloride [52,53] and even phosphate. The effect of adding chloride is demonstrated in Fig.…”

Section: Electrocatalytic Glucose Oxidationmentioning

confidence: 99%

High-Utilisation Nanoplatinum Catalyst (Pt@cPIM) Obtained via Vacuum Carbonisation in a Molecularly Rigid Polymer of Intrinsic Microporosity

Rong

Malpass‐Evans

et al. 2016

Electrocatalysis

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Polymers of intrinsic microporosity (PIM or here PIM-EA-TB) offer a highly rigid host environment into which hexachloroplatinate(IV) anions are readily adsorbed and vacuum carbonised (at 500°C) to form active embedded platinum nanoparticles. This process is characterised by electron and optical microscopy, atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and electrochemical methods, which reveal that the PIM microporosity facilitates the assembly of nanoparticles of typically 1.0 to 2.5-nm diameter. It is demonstrated that the resulting carbonised BPt@cPIM^from drop-cast films of ca. 550-nm average thickness, when prepared on tin-doped indium oxide (ITO), contain not only fully encapsulated but also fully active platinum nanoparticles in an electrically conducting heterocarbon host. Alternatively, for thinner films (50-250 nm) prepared by spin coating, the particles become more exposed due to additional loss of the carbon host. In contrast to catalyst m a t e r i a l s p r e p a r e d b y v a c u u m-t h e r m o l y s e d hexachloroplatinate(IV) precursor, the platinum nanoparticles within Pt@cPIM retain high surface area, electrochemical activity and high catalyst efficiency due to the molecular rigidity of the host. Data are presented for oxygen reduction, methanol oxidation and glucose oxidation, and in all cases, the high catalyst surface area is linked to excellent catalyst utilisation. Robust transparent platinum-coated electrodes are obtained with reactivity equivalent to bare platinum but with only 1 μg Pt cm −2 (i.e.~100% active Pt nanoparticle surface is maintained in the carbonised microporous host).

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“…The oxidation of glucose on platinum is known to be very sensitive to poisons such as chloride [52,53] and even phosphate. The effect of adding chloride is demonstrated in Fig.…”

Section: Electrocatalytic Glucose Oxidationmentioning

confidence: 99%

High-Utilisation Nanoplatinum Catalyst (Pt@cPIM) Obtained via Vacuum Carbonisation in a Molecularly Rigid Polymer of Intrinsic Microporosity

Rong

Malpass‐Evans

et al. 2016

Electrocatalysis

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“…For the bare platinum (trace i) characteristic signals for platinum oxidation (broad anodic feature at 0.2 to 0.8 V vs. SCE) and back reduction (cathodic peak at 0.0 V vs. SCE) are observed. In the negative potential range two peaks denoted Process 1 and Process 2 are observed consistent (at least in first approximation) with the formation of weakly and strongly adsorbed hydrogen, respectively (see equation 1 and .

true Process 1 : normalH^{+} (aq) + normale^{-} (Pt) \vec{\leftarrow} Pt - normalH (strong)

true Process 2 : normalH^{+} (aq) + normale^{-} (Pt) \vec{\leftarrow} Pt - normalH (weak)

…”

Section: Resultsmentioning

confidence: 99%

Triphasic Nature of Polymers of Intrinsic Microporosity Induces Storage and Catalysis Effects in Hydrogen and Oxygen Reactivity at Electrode Surfaces

et al. 2018

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Hydrogen oxidation and oxygen reduction are two crucial energy conversion reactions, which are shown to be both strongly affected by the presence of intrinsically microporous polymer coatings on electrodes. Polymers of intrinsic microporosity (PIMs) are known to possess extremely high internal surface area and ability to bind gases under dry conditions. It is shown here that both, hydrogen‐ and oxygen gas binding into PIMs, also occurs under wet or “triphasic” conditions in aqueous electrolyte environments (when immersed in 0.01 M phosphate buffer at pH 7). For two known PIM materials (PIM‐1 and PIM‐PY), nanoparticles are formed by an anti‐solvent precipitation protocol and then cast as a film onto platinum or glassy carbon electrodes. Voltammetry experiments reveal evidence for hydrogen and oxygen binding. Both, PIM‐1 and PIM‐PY, locally store hydrogen or oxygen gas at the electrode surface and thereby significantly affect electrocatalytic reactivity. The onset of oxygen reduction on glassy carbon is shifted by 0.15 V in the positive direction.

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“…Identification of characteristic hydrogen underpotential adsorption peaks [ 36 ] was not possible in acidic aqueous solution due to a high charging current generated by the capacitive nature of the cPIM-electrolyte interface. The presence of excess protons is believed to increase the double layer capacitance [ 9 ].…”

Section: Resultsmentioning

confidence: 99%

Platinum Nanoparticle Inclusion into a Carbonized Polymer of Intrinsic Microporosity: Electrochemical Characteristics of a Catalyst for Electroless Hydrogen Peroxide Production

et al. 2018

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The one-step vacuum carbonization synthesis of a platinum nano-catalyst embedded in a microporous heterocarbon (Pt@cPIM) is demonstrated. A nitrogen-rich polymer of an intrinsic microporosity (PIM) precursor is impregnated with PtCl62− to give (after vacuum carbonization at 700 °C) a nitrogen-containing heterocarbon with embedded Pt nanoparticles of typically 1–4 nm diameter (with some particles up to 20 nm diameter). The Brunauer-Emmett-Teller (BET) surface area of this hybrid material is 518 m2 g−1 (with a cumulative pore volume of 1.1 cm3 g−1) consistent with the surface area of the corresponding platinum-free heterocarbon. In electrochemical experiments, the heterocarbon-embedded nano-platinum is observed as reactive towards hydrogen oxidation, but essentially non-reactive towards bigger molecules during methanol oxidation or during oxygen reduction. Therefore, oxygen reduction under electrochemical conditions is suggested to occur mainly via a 2-electron pathway on the outer carbon shell to give H2O2. Kinetic selectivity is confirmed in exploratory catalysis experiments in the presence of H2 gas (which is oxidized on Pt) and O2 gas (which is reduced on the heterocarbon surface) to result in the direct formation of H2O2.

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Electrothermal Annealing of Catalytic Platinum Microwire Electrodes: Towards Membrane‐Free pH 7 Glucose Micro‐Fuel Cells

Cited by 6 publications

References 27 publications

High-Utilisation Nanoplatinum Catalyst (Pt@cPIM) Obtained via Vacuum Carbonisation in a Molecularly Rigid Polymer of Intrinsic Microporosity

High-Utilisation Nanoplatinum Catalyst (Pt@cPIM) Obtained via Vacuum Carbonisation in a Molecularly Rigid Polymer of Intrinsic Microporosity

Triphasic Nature of Polymers of Intrinsic Microporosity Induces Storage and Catalysis Effects in Hydrogen and Oxygen Reactivity at Electrode Surfaces

Platinum Nanoparticle Inclusion into a Carbonized Polymer of Intrinsic Microporosity: Electrochemical Characteristics of a Catalyst for Electroless Hydrogen Peroxide Production

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