The voltammetry of decamethylferrocene and coboltacene in supercritical difluoromethane (R32)

Bartlett, Philip N.; Branch, Jack A.

doi:10.1016/j.jelechem.2016.09.043

Cited by 4 publications

(4 citation statements)

References 45 publications

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“…Natural convection driven by thermal or density gradients is much more significant in supercritical fluids than in conventional liquid electrolytes because of the much lower viscosity of the supercritical fluid. As we have shown in our earlier studies [33][34][35] this manifests itself as noise in the mass transport limited current at microelectrodes and distortion of slow scan rate cyclic voltammetry. As can be seen from Figure 8 the voltammetry obtained in the plastic reactor shows well defined features with little to no intrinsic convection, even at scan rates of 10 mV/s.…”

Section: Voltammetry Of Decamethylferrocenementioning

confidence: 63%

“…An alternative, although not an ideal solution, is to use an outer sphere redox couple as an internal redox standard and decamethylferrocene (DMFc) has been shown to be a suitable choice for used in supercritical difluoromethane (scR32). 33 In the present case we have used the stainless steel body of the thermocouple as a pseudo reference electrode. It would also be possible to electroplate the thermocouple body with Pt or another metal and use this as a pseudo reference electrode or to incorporate a pseudo reference electrode, or other type of reference electrode, in one of the top or bottom electrode structures.…”

Section: Methodsmentioning

confidence: 99%

“…In the literature pseudo reference electrodes are almost always used20,[29][30][31][32] even though they have obvious limitations. An alternative, although not an ideal solution, is to use an outer sphere redox couple as an internal redox standard and decamethylferrocene (DMFc) has been shown to be a suitable choice for used in supercritical difluoromethane (scR32) 33. In the present case…”

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confidence: 93%

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Plastic Reactor Suitable for High Pressure and Supercritical Fluid Electrochemistry

Branch

Alibouri

Cook

et al. 2017

J. Electrochem. Soc.

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The paper describes a reactor suitable for high pressure, particularly supercritical fluid, electrochemistry and electrodeposition at pressures up to 30 MPa at 115 • C. The reactor incorporates two key, new design concepts; a plastic reactor vessel and the use of o-ring sealed brittle electrodes. These two innovations widen what can be achieved with supercritical fluid electrodeposition. The suitability of the reactor for electroanalytical experiments is demonstrated by studies of the voltammetry of decamethylferrocene in supercritical difluromethane and for electrodeposition is demonstrated by the deposition of Bi. The application of the reactor to the production of nanostructures is demonstrated by the electrodeposition of ∼80 nm diameter Te nanowires into an anodic alumina on silicon template. Key advantages of the new reactor design include reduction of the number of wetted materials, particularly glues used for insulating electrodes, compatability with reagents incompatible with steel, compatability with microfabricated planar multiple electrodes, small volume which brings safety advantages and reduced reagent useage, and a significant reduction in experimental time.

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Section: Voltammetry Of Decamethylferrocenementioning

confidence: 63%

Section: Methodsmentioning

confidence: 99%

mentioning

confidence: 93%

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Plastic Reactor Suitable for High Pressure and Supercritical Fluid Electrochemistry

Branch

Alibouri

Cook

et al. 2017

J. Electrochem. Soc.

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“…In both cases the current rises to a plateau at negative potentials. In the case of the bare TiN electrode, this plateau shows significant noise due to convection in the cell . For the mesoporous silica-coated electrode the voltammetry follows the expected pattern with a peak on the cathodic scan at around −1.8 V as the tin complex within the template is consumed and then a plateau at lower current density on the return cycle corresponding to diffusion of the tin complex across the mesoporous silica film.…”

mentioning

confidence: 77%

Exploration of the Smallest Diameter Tin Nanowires Achievable with Electrodeposition: Sub 7 nm Sn Nanowires Produced by Electrodeposition from a Supercritical Fluid

et al. 2018

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Electrodeposition of Sn from supercritical difluoromethane has been performed into anodic alumina templates with pores down to 3 nm in diameter and into mesoporous silica templates with pores of diameter 1.5 nm. Optimized deposits have been characterized using X-ray diffraction, scanning electron microscopy, and scanning transmission electron microscopy (bright field, high-angle annular dark field, and energy-dispersive X-ray elemental mapping). Crystalline 13 nm diameter Sn nanowires have been electrodeposited in symmetric pore anodic alumina. Direct transmission electron microscopy evidence of sub 7 nm Sn nanowires in asymmetric anodic alumina has been obtained. These same measurements present indirect evidence for electrodeposition through 3 nm constrictions in the same templates. A detailed transmission electron microscopy study of mesoporous silica films after Sn deposition is presented. These indicate that it is possible to deposit Sn through the 1.5 nm pores in the mesoporous films, but that the nanowires formed are not stable. Suggestions of why this is the case and how such extreme nanowires could be stabilized are presented.

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(Bio)electroanalysis in the Field of Greener Analytical Chemistry

Yáñez‐Sedeño

Campuzano

Pingarrón

2020

Challenges in Green Analytical Chemistry

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Modern (bio)electroanalysis is currently in consonance with the demands of green chemistry owing to both the intrinsic characteristics of electrochemical transduction and the unique features offered by electrochemical devices to minimize the use of reagents, organic solvents and hazardous substances. Remarkable efforts have been made in recent years in the preparation of modified electrode substrates involving non-toxic materials and greener protocols, more biological than chemical, to perform the electrochemical measurements or pretreat the sample. It is also notable in this context the particular attention that has been paid to the development of environmentally friendly electrochemical sensors involving paper, molecularly imprinted polymers and ion-selective electrodes. In addition, the replacement of organic solvents by eco-friendly solvents (ionic liquids, deep eutectic solvents and supercritical fluids) and the growing interest in developing methodologies capable of reducing the sample size and the amount of waste products, mainly by miniaturization of the electrochemical approaches and their coupling with continuous techniques, are novel approaches to be considered in green electroanalysis. All these relevant aspects are discussed and illustrated in this chapter through a critical approach to representative studies selected from the recent literature.

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The voltammetry of decamethylferrocene and coboltacene in supercritical difluoromethane (R32)

Cited by 4 publications

References 45 publications

Plastic Reactor Suitable for High Pressure and Supercritical Fluid Electrochemistry

Plastic Reactor Suitable for High Pressure and Supercritical Fluid Electrochemistry

Exploration of the Smallest Diameter Tin Nanowires Achievable with Electrodeposition: Sub 7 nm Sn Nanowires Produced by Electrodeposition from a Supercritical Fluid

(Bio)electroanalysis in the Field of Greener Analytical Chemistry

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