Cathodic fabrication of platinum microparticles via anodic dissolution of a platinum counter-electrode: Electrocatalytic probing and surface analysis of dispersed platinum

Kulesza, Paweł J.; Lu, Wenyuan; Faulkner, Larry R.

doi:10.1016/0022-0728(92)80260-b

Cited by 42 publications

(30 citation statements)

References 30 publications

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“…However, one needs to consider that the CE potential is free floating and the applied CE potential under fast cycling can change between very high and low values. Under these conditions severe Pt dissolution can take place and in the worst case Pt ions can redeposit onto the catalyst at the WE [23,24].…”

Section: Approaches For Half-cell Degradation Studies 21 Experimentamentioning

confidence: 99%

Fuel cell catalyst degradation: Identical location electron microscopy and related methods

Arenz

Zana

2016

Nano Energy

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Fuel cells are an important piece in our quest for a sustainable energy supply. Although there are several different types of fuel cells, the by far most popular is the proton exchange membrane fuel cell (PEMFC). Among its many favorable properties are a short start up time and a high power density; both essential for automotive applications. Its drawback is the use of carbon supported Pt or Pt alloys as the active catalyst. The scarce resources of Pt led to significant efforts in reducing the amount of Pt used in PEMFCs. Thanks to the advancements of these efforts, catalyst stability gained increasing focus. Activity of the catalyst is important, but stability is essential. In the presented perspective paper, we review recent efforts to investigate fuel cell catalysts ex-situ in electrochemical half-cell measurements. Due to the amount of different studies, this review has no intention to give a complete overview and cover all studies. Instead we concentrate on efforts of our and other research groups to apply identical location electron microscopy and related methods to study the degradation of PEMFC catalysts.

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Section: Approaches For Half-cell Degradation Studies 21 Experimentamentioning

confidence: 99%

Fuel cell catalyst degradation: Identical location electron microscopy and related methods

Arenz

Zana

2016

Nano Energy

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“…12,14,[16][17][18][19][20] Dissolved Pt ions can reach and become deposited on the electrocatalyst surface, increasing the apparent activity of the test material. 3,7,8,12,[21][22][23][24][25][26] Increasing the surface area of the counter electrode decreases the current density it experiences, and while this can slow the dissolution process, it cannot stop it. 27 Dissolved Clions (either from the supporting electrolyte or leaking from a reference electrode) can also increase the rate of dissolution of Pt and Au electrodes through the formation of metal-chloride complexes.…”

Section: Introductionmentioning

confidence: 99%

Best Practice for Evaluating Electrocatalysts for Hydrogen Economy

Bird

Goodwin

Walsh

2020

ACS Appl. Mater. Interfaces

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Screening new electrocatalysts is key to the development of new materials for next-generation energy devices such as fuel cells and electrolysers. The counter electrodes used in such tests are often made from materials such as Pt and Au, which can dissolve during testing and deposit onto test electrocatalysts, resulting in inaccurate results. The most common strategy for preventing this effect is to separate the counter electrode from the test material using an ion-transporting Nafion membrane. Here, we use X-ray photoelectron spectroscopy, energy-dispersive X-ray analysis, mass spectrometry, and voltammetry to demonstrate the limitations of this approach during constant-current, extended stability testing of electrocatalysts for H2 evolution. We show that Nafion membranes cannot prevent contamination of carbon electrocatalysts by Pt and Au counter electrodes, leading to an apparent increase in electrocatalytic activity of the carbon. We then demonstrate that carbon counter electrodes in undivided cells can contaminate and deactivate Pt and Au electrocatalysts for H2 evolution. We show that use of a setup comprising a glass frit separating a carbon counter electrode from the test electrocatalyst can prevent these effects. Finally, we discuss these phenomena using H2 evolution at MoS2 and at a K6[P2W18O62](H2O)14/carbon nanotube composite as test reactions.

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“…The presence of chlorides facilitated anodic dissolution of platinum [45]. It should be stressed that under our experimental conditions, in applied potential window, platinum was neither deposited when the carbon paper was employed as the counter electrode [43,44] nor when KCl was absent in the electrolyte. Following deposition of platinum, an electrode covered with the catalytic layer (Pt-Cs 2.5 H 0.5 PW 12 O 40 /Vulcan or Pt-Vulcan) was washed out with water and subjected to cycling in 0.5 mol dm −3 H 2 SO 4 in the potential range from 0 to 1.05 V vs. RHE to remove Cl − from the catalytic film.…”

Section: Methodsmentioning

confidence: 97%

“…In the present work, we describe a unique preparation method and discuss electrocatalytic properties (towards oxygen reduction and hydrogen oxidation) of composite utilizing the Cs 2.5 H 0.5 PW 12 O 40 salt functioning as stable and active matrix for highly dispersed platinum nanocenters (at ultratrace level) obtained via anodic dissolution (corrosion) of the platinu m counter elec trode [13,[42][43][44]. Since heteropolytungstates are better catalysts for reduction of oxygen than their molybdenum counterparts [20][21][22], we have focused here exclusively on the tungsten-containing compound.…”

Section: Introductionmentioning

confidence: 99%

Electrocatalytic properties of platinum nanocenters electrogenerated at ultra-trace levels within zeolitic phosphododecatungstate cesium salt matrices

Kolary-Zurowska

Zurowski

Dsoke

et al. 2014

J Solid State Electrochem

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A unique preparation method of obtaining stable composite film (with ultra-low platinum content) highly active towards oxygen reduction and hydrogen oxidation is presented here. The matrix for platinum centers consists of highsurface-area zeoli te-t ype aci dic salt of cesium phosphododecatungstate (Cs 2.5 H 0.5 PW 12 O 40 ) admixed with carbon (Vulcan XC-72) carriers. Platinum nanoparticles were deposited on the working electrode modified with matrix via corrosion of platinum counter electrode during cyclic voltammetry experiment conducted in acid electrolyte containing chloride ions. The results obtained from rotating disk voltammetry revealed that the composite film containing Pt nanoparticles at very low loadings (on the level of 2-5 μg cm −2 ) demonstrated remarkable electrocatalytic activity towards both oxygen reduction and hydrogen oxidation, particularly, when compared to the performance of the Cs 2.5 H 0.5 PW 12 O 40 -free system (i.e., containing only Vulcan support) prepared and examined under analogous conditions. The phenomenon should be primarily ascribed to the mesoporous nature of the matrix enabling immobilization and stabilization of small catalytic nanoparticles (1-2 nm diameters) inside the pores as well as to high surface acidity of the polyoxometalate-based salt providing proton-rich environment at the electrocatalytic interface.

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Cathodic fabrication of platinum microparticles via anodic dissolution of a platinum counter-electrode: Electrocatalytic probing and surface analysis of dispersed platinum

Cited by 42 publications

References 30 publications

Fuel cell catalyst degradation: Identical location electron microscopy and related methods

Fuel cell catalyst degradation: Identical location electron microscopy and related methods

Best Practice for Evaluating Electrocatalysts for Hydrogen Economy

Electrocatalytic properties of platinum nanocenters electrogenerated at ultra-trace levels within zeolitic phosphododecatungstate cesium salt matrices

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