Electrochimica Acta 76 (2012) 389–393
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Electrochimica Acta
jou rn al hom epa ge: www.elsevier.com/locate/electacta
The high throughput electrochemical screening of the corrosion resistance of
Ni–Cr thin film alloys
Talal A. Aljohani, Brian E. Hayden
∗
, Alexandros Anastasopoulos
Department of Chemistry, University of Southampton, Southampton SO17 1BJ, United Kingdom
a r t i c l e i n f o
Article history:
Received 19 March 2012
Received in revised form 9 May 2012
Accepted 10 May 2012
Available online 17 May 2012
Keywords:
Corrosion
High throughput
Polarisation resistance
PVD
Thin films
Ni–Cr alloys
a b s t r a c t
The corrosion behaviour of a series of NiCr thin film alloys were characterised through the high-
throughput electrochemical measurement of their polarisation resistance on a micro-fabricated array
of electrodes. The linear polarisation resistance (LPR) method has been compared to the results from
Tafel extrapolation, and the alloy compositional dependence of the polarisation resistance as a function
of composition is consistent. There are, however, some systematic differences in the absolute values
extracted using the two methodologies which are likely to be a result of the smaller current densities
associated with the LPR method. In the case of the NiCr alloys deposited at 300 K, the observed bulk
phases closely agree with those expected from the literature. The polarisation resistance behaviour is
shown to be directly related to the bulk alloy structures. Besides the b.c.c. -Cr(Im3m) phase and its Ni
solid solutions which exhibit the highest polarisation resistances, the -Cr
3
Ni
2
(P4
2
/mnm) phase exhibits
the next best polarisation resistance, and its co-existence with the -Cr
7
Ni
3
(P4
2
/mnm) phase at higher
Cr content results in a lowering of that resistance.
© 2012 Elsevier Ltd. All rights reserved.
1. Introduction
Combinatorial or high-throughput methods have been widely
applied to the screening and optimisation of metal alloy [1] and
supported metal nano-particle electrocatalysts [2]. Recently, the
combinatorial approach has been implemented for the purpose of
investigating the corrosion behaviour of materials [3,4]. A scan-
ning droplet cell [5] was successfully employed to investigate the
passivation behaviour of some thin film alloys [3,6–8]. A optical
screening method has been used to assess corrosion behaviour of
library of thin films by image analysis of electrodes before and
after exposure to the corrosion environment [4]. A multi-electrode
method has been applied to evaluate corrosion behaviour before
and after adding inhibitors: Pairs of identical wires embedded in
an insulator are interrogated by applying potentials which activate
both anodic and cathodic responses [9,10].
In the present study we have adapted the high throughput
screening methodology employing multi-channel current follow-
ers [11] and a silicon micro-fabricated array of independently
addressable electrodes [1] to the screening of corrosion char-
acteristics of thin film materials. The screening methodology is
compatible with the high-throughput PVD methodology based
on MBE sources [12] allowing the controllable deposition of
∗
Corresponding author. Tel.: +44 02380592776; fax: +44 02380593781.
E-mail address: beh@soton.ac.uk (B.E. Hayden).
compositional gradients of a large range of thin film materials. The
method has been applied to the study of a library of Ni–Cr alloys in
order to assess the effectiveness of this high-throughput approach.
2. Experimental
Ni–Cr binary alloy thin films were prepared using a High
Throughput Physical Vapour Deposition (HT-PVD) method
described in detail elsewhere [12]. A compositional gradient of
the alloy was synthesised by simultaneously depositing the two
elements Cr (Alfa Aesar 99.99% purity) and Ni (Alfa Aesar 99.95%
purity) from electron beam sources with the substrate at 300 K,
allowing the complete mixing of elements (kinetically controlled),
minimising surface segregation and eliminating any need for
post-deposition annealing. The cryo-pumped UHV chamber had
a base pressure of 1 × 10
-10
mbar. The two e-beam sources were
arranged in a 120
◦
geometry. Thin films were deposited on two
substrates. A 32 mm
2
silicon/silicon nitride substrates (Nova
Electronic Materials) were employed for X-ray diffraction (XRD)
using a Bruker D8 powder diffractometer with a C2 area detec-
tor. A (10 × 10) silicon micro-fabricated array of independently
addressable working electrodes (Ilika Technologies Ltd.) was used
for the high throughput combinatorial electrochemical screening
of the alloys. Composition analysis by Electron Dispersive X-ray
Spectroscopy (EDS) using a JEOL JSM5910 and Oxford Instruments
INCA 300 was also carried out on these substrates. Details regard-
ing the design and fabrication of these arrays, and the principles
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http://dx.doi.org/10.1016/j.electacta.2012.05.045