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Bipolar electrochemistry for high throughput screening applications
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Chemistry - Ångström, Structural Chemistry.
2016 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Bipolar electrochemistry is an interesting concept for high throughput screening techniques due to the ability to induce gradients in a range of materials and their properties, such as composition, particle size, or dopant levels, among many others. One of the key advantages of the method is the ability to test, create or modify materials without the need for a direct electrical connection. In this thesis, the viability of this method has been explored for a range of possible applications, such as metal recycling, nanoparticle modification and corrosion analysis.

In the initial part of the work a process to electrodeposit gradients in metal composition was evaluated, with a view to applying the technique to the extraction and recycling of metals from fly ash. Compositional gradients in the metals under study could be readily obtained from controlled reference solutions, although the spatial resolution of the metals was not sufficient to perform separation. Only copper could be easily deposited from the fly ash solution.

Bipolar electrodeposition was also successfully used to modify the particle size across substrates decorated with gold nanoparticles. The approach was demonstrated both for surfaces possessing either a uniform particle density or a gradient in particle density. In the latter case samples with simultaneous, orthogonal gradients in both particle size and density were obtained.

A combination of the bipolar approach with rapid image analysis was also evaluated as a method for corrosion screening, using quantitative analysis of gradients in pitting corrosion damage on stainless steels in HCl as a model system. The factors affecting gradient formation and the initiation of corrosion were thoroughly investigated by the use of a scanning droplet cell (SDC) technique and hard x-ray photoelectron spectroscopy (HAXPES). The ability to screen arrays of different materials for corrosion properties was also investigated, and demonstrated for stainless steel and Ti-Al alloys with pre-formed compositional gradients. The technique shows much promise for further studies and for high throughput corrosion screening applications.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis, 2016. , 77 p.
Series
Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1651-6214 ; 1348
Keyword [en]
bipolar electrochemistry, electrodeposition, corrosion, screening, gradients, recycling, gold nanoparticles, Scanning Droplet Cell, Hard x-ray photoelectron spectroscopy, pitting corrosion
National Category
Chemical Sciences
Research subject
Chemistry with specialization in Materials Chemistry
Identifiers
URN: urn:nbn:se:uu:diva-277937ISBN: 978-91-554-9491-9 (print)OAI: oai:DiVA.org:uu-277937DiVA: diva2:907117
Public defence
2016-04-15, Häggsalen, Ångströmlaboratoriet, Lägerhyddsvägen 1, Uppsala, 09:15 (English)
Opponent
Supervisors
Available from: 2016-03-23 Created: 2016-02-23 Last updated: 2016-04-04
List of papers
1. Bipolar electrodeposition of heavy metal compositional gradients
Open this publication in new window or tab >>Bipolar electrodeposition of heavy metal compositional gradients
(English)Manuscript (preprint) (Other (popular science, discussion, etc.))
National Category
Materials Chemistry
Identifiers
urn:nbn:se:uu:diva-277942 (URN)
Available from: 2016-02-26 Created: 2016-02-23 Last updated: 2016-04-04
2. Formation of Gold Nanoparticle Size and Density Gradients via Bipolar Electrochemistry
Open this publication in new window or tab >>Formation of Gold Nanoparticle Size and Density Gradients via Bipolar Electrochemistry
Show others...
2016 (English)In: ChemElectroChem, ISSN 2196-0216, Vol. 3, no 3, 378-382 p.Article in journal (Refereed) Published
Abstract [en]

Bipolar electrochemistry is employed to demonstrate the formation of gold nanoparticle size gradients on planar surfaces. By controlling the electric field in a HAuCl4-containing electrolyte, gold was reduced onto 10 nm diameter particles immobilized on pre-modified thiolated bipolar electrode (BPE) templates, resulting in larger particles towards the more cathodic direction. As the gold deposition was the dominating cathodic reaction, the increased size of the nanoparticles also reflected the current distribution on the bipolar electrode. The size gradients were also combined with a second gradient-forming technique to establish nanoparticle surfaces with orthogonal size and density gradients, resulting in a wide range of combinations of small/large and few/many particles on a single bipolar electrode. Such surfaces are valuable in, for example, cell-material interaction and combinatorial studies, where a large number of conditions are probed simultaneously.

National Category
Chemical Sciences Materials Chemistry
Identifiers
urn:nbn:se:uu:diva-277930 (URN)10.1002/celc.201500413 (DOI)000372296100006 ()
Funder
Swedish Research Council Formas, 2010-1572Swedish Research Council, 2009-5398
Available from: 2016-02-26 Created: 2016-02-23 Last updated: 2017-01-25Bibliographically approved
3. Bipolar electrochemistry for high-throughput corrosion screening
Open this publication in new window or tab >>Bipolar electrochemistry for high-throughput corrosion screening
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2013 (English)In: Electrochemistry communications, ISSN 1388-2481, E-ISSN 1873-1902, Vol. 34, 274-277 p.Article in journal (Refereed) Published
Abstract [en]

It is demonstrated that bipolar electrochemistry can be used for high-throughput corrosion testing covering a wide potential range in one single experiment and that this, combined with rapid image analysis, constitutes a simple and convenient way to screen the corrosion behaviour of conducting materials and corrosion protective coatings. Stainless steel samples (SS304), acting as bipolar electrodes, were immersed in sulphuric and hydrochloric acid and exposed to an electric field to establish a potential gradient along the surface. In this way, the same steel sample was exposed to a wide range of cathodic and anodic conditions, ranging from potentials yielding hydrogen evolution to potentials well into the transpassive region. This wireless approach enables rapid simultaneous comparison of numerous samples, and also provides the opportunity to perform experiments on samples that are of a complex shape, or which otherwise are difficult to employ in standard electrochemical corrosion tests.

Keyword
Bipolar electrochemistry, Corrosion, Stainless steel, Screening, Image analysis
National Category
Materials Chemistry Inorganic Chemistry
Research subject
Materials Science
Identifiers
urn:nbn:se:uu:diva-205921 (URN)10.1016/j.elecom.2013.07.011 (DOI)000324963900070 ()
Note

Highlights

• Bipolar electrochemistry for high-throughput corrosion screening

• Simultaneous evaluation of anodic and cathodic conditions on single samples

• Wireless production of corrosion gradients on stainless steel and image analysis

• Comparison of the bipolar approach with conventional three-electrode experiments

Available from: 2013-08-25 Created: 2013-08-25 Last updated: 2017-12-06Bibliographically approved
4. Spatially resolved electrochemical and surface analysis of bipolar-induced corrosion gradients
Open this publication in new window or tab >>Spatially resolved electrochemical and surface analysis of bipolar-induced corrosion gradients
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(English)Manuscript (preprint) (Other academic)
National Category
Materials Chemistry
Identifiers
urn:nbn:se:uu:diva-278883 (URN)
Available from: 2016-02-26 Created: 2016-02-26 Last updated: 2016-04-04
5. Towards high throughput corrosion screening using arrays of bipolar electrodes
Open this publication in new window or tab >>Towards high throughput corrosion screening using arrays of bipolar electrodes
2015 (English)In: JOURNAL OF ELECTROANALYTICAL CHEMISTRY, ISSN 1572-6657, Vol. 747, 77-82 p.Article in journal (Refereed) Published
Abstract [en]

In this work we demonstrate the possibility of combining bipolar electrochemistry with arrays of samples as a fast and versatile method for comparing their corrosion resistances at a wide range of potentials. Several steel samples of different grades were arranged in a bipolar electrochemical cell and exposed to an electric field by applying a constant current. The gradient in electrochemical potential difference across each sample resulted in a pitting corrosion gradient on the anodic parts which was used as a simple, straightforward and qualitative method of screening the corrosion properties of several samples in one single experiment. In the cell, all samples acted as individual bipolar electrodes but interestingly, the current density for each sample was also found to be influenced by the corrosion resistances of its neighbours. Results from the bipolar array were also compared with standard polarisation curves and the pitting resistance equivalent number (PREN) for each steel type.

Keyword
Bipolar electrochemistry, Corrosion screening, Pitting corrosion, Surface gradients, Stainless steel
National Category
Chemical Sciences
Identifiers
urn:nbn:se:uu:diva-257641 (URN)10.1016/j.jelechem.2015.04.008 (DOI)000355711000010 ()
Available from: 2015-07-09 Created: 2015-07-06 Last updated: 2016-04-04Bibliographically approved

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