Sensors and Actuators A 223 (2015) 91–96

Contents lists available at ScienceDirect

Sensors and Actuators A: Physical

journal homepage: www.elsevier.com/locate/sna

Optimised co-electrodeposition of Fe–Ga alloys for maximum

magnetostriction effect
Jack H.-G. Ng, Paul M. Record, Xinxin Shang, Krystian L. Wlodarczyk, Duncan P. Hand,
Giuseppe Schiavone ∗ , Eitan Abraham, Gerard Cummins, Marc P.Y. Desmulliez
School of Engineering and Physical Sciences, Heriot-Watt University, Edinburgh EH14 4AS, UK

a r t i c l e i n f o a b s t r a c t

Article history: The article reports the electrochemical deposition and characterisation of a 600 nm thick Fe–Ga alloy
Received 2 September 2014 film plated on a 20 ␮m thick copper cantilever. The co-electrodeposition process was optimised for the
Received in revised form production of Fe–Ga in the ratio of 81% Fe to 19% Ga, which is known to maximize the magnetostriction
21 November 2014
(MS) effect. The foil was cut into 1 mm wide and 5 mm long cantilevers and the deflection was measured
Accepted 11 December 2014
with DC co-planar magnetic field intensities ranging from 0 to 60 kA/m. The maximum strain coefficient
Available online 3 January 2015
 was measured to be 96 ppm for a field strength range 58 kA/m. The field strain plot over exhibits a
typical second order magnetically induced strain curve, as seen in other magnetostrictive materials.
Keywords:
Galfenol © 2014 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY license
Magnetostriction (http://creativecommons.org/licenses/by/4.0/).
Electrodeposition
Magnetic actuation
Magnetostrictive coefficient
Alloy electrodeposition

1. Introduction and the production of nanowires [9], demonstrating the viabil-

ity of this method for large-scale production of magnetostrictive
Magnetostriction is defined as the ability of a material to expe- microstructures and MEMS devices [7,8].
rience mechanical strain when subject to a magnetic field. The There are several challenges associated with the electrodeposi-
material with the highest known strain coefficient of magnetostric- tion process of galfenol films [4,6]. There are only a few pH–voltage
tion,  ∼ 2000 ppm, is currently Terfenol-D, an alloy of terbium, combinations where Ga ions remain stable in aqueous solutions
dysprosium and iron (Tb0.3 Dy0.7 Fe2 ) that has poor ductility and low [6] Other challenges include hydrogen evolution due to the high
fracture resistance making it difficult to machine [1,2]. Galfenol, an electrolyte pH that leads to gallium hydroxide and oxide being
alloy of iron and gallium (Fe0.8 Ga0.2 ) is easily machined and offers formed and included in the deposits [4–6]. A combinatorial study
good  ∼ 275–320 ppm at relatively low field strengths (39 kA/m) by McGary [6] where a Hull Cell was used to vary the current
[3]. This material also exhibits high tensile strength and can be density across the cathode showed that the use of complexing
used in tension unlike Terfenol-D. However high temperature and agents such as sodium citrate reduces the oxygen content of the
pressure are required to manufacture this alloy. Galfenol may also electrodeposited material. More recent work by Iselt [4] achieved
be deposited by sputtering though this manufacturing technique significantly low oxygen content through the use of alternating
requires expensive vacuum equipment and the deposition rate potential pulses.
depends on the partial pressure of the inert gas [1]. This work is extended in this article by optimisation of the
Recently work has been published on a method of electrochem- electroplating process using a previously reported electrolyte bath
ically depositing Galfenol [4–9]. Electrodeposition of Galfenol has composition [9]. Characterisation of the resulting deposits onto
many advantages over previous methods of deposition, such as 20 ␮m thick copper cantilever beams reveals that two alloys,
low cost, high deposition rate and the ability to coat large or non- Fe0.81 Ga0.19 and Fe0.71 Ga0.29 , that display large magnetostructive
planar surfaces. This method can be used for thin film deposition coefficients have been successfully electro-deposited [1].

2. Plating development
∗ Corresponding author. Tel.: +44 0 131 451 8315; fax: +44 0 131 451 4155.
E-mail addresses: giu.schiavone@gmail.com, g.schiavone@hw.ac.uk Co-deposition of Fe–Ga alloys from a simple, single aqueous
(G. Schiavone). electrolyte involves a complex deposition mechanism comprising

http://dx.doi.org/10.1016/j.sna.2014.12.014
0924-4247/© 2014 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
92 J.H.-G. Ng et al. / Sensors and Actuators A 223 (2015) 91–96

Table 1
Aqueous electrolyte for Fe–Ga electrodeposition.

Component Concentration (M)

Ga2 (SO4 )3 ·18H2 O 0.06

FeSO4 ·7H2 O 0.03
H3 BO3 0.5
Na3 C6 H5 O7 0.15
C6 H8 O6 0.04

electrochemical and chemical deposition processes [4–6]. Dense,

homogeneous and oxygen free films are obtained by applying
alternating potential pulses [4]. This section describes the devel-
opment of the plating process and elemental characterisation of
the deposits.
Fig. 1. Ratio of gallium content over the total Fe + Ga deposit as a function of con-
centration of Fe2+ ions in the co-deposition electrolyte system as measured by EDX.
2.1. Method

The starting aqueous electrolytes contain 0.06 M Ga2 (SO4 )3 · of the Ga3+ ions relative to the Fe2+ ions in the co-deposition
18H2 O and 0.03 M FeSO4 ·7H2 O as the Fe and Ga sources, respec- electrolyte system [5]. In this article, a further reduction of the
tively. 0.5 M boric acid and 0.15 M sodium citrate are added as concentration of the Fe2+ ions is reported for the plating of large
buffer and 0.04 M ascorbic acid acts as an antioxidant [4,5]. The pH is structures, such as the millimetre size cantilevers described later.
adjusted to less than 3.0 with dilute H2 SO4 to avoid gallium hydrox- The concentration of Fe2+ ions in the plating bath has a dominant
ide precipitation. The iron sulphate concentration was reduced in effect on the Ga:Fe ratio of the resultant solid deposit. As shown
subsequent experiments in order to obtain the desired Fe:Ga ratio in Fig. 1 the reduction of the concentration of Fe2+ ions and the
in the electrodeposits. Table 1 summarises the initial electrolyte increase of the pH result in a significant increase of the gallium
composition for a total volume of 50 mL. content in the deposit. An appreciable amount of gallium deposit
Electrodeposition experiments were performed with 50 mL of is only achieved when the Fe2+ ions concentration is reduced to
the electrolyte in a rectangular electrolytic cell with a three- 1/5 (0.006 M) or below of the recipe suggested by Iselt et al. [5].
electrode system in conjunction with a DropSense ␮Stat 400 Secondly, the suggested pH value of slightly less than 3.0 from the
potentiostat/galvanostat. A large surface area platinum mesh was literature does not allow significant gallium deposition until the
used as the counter electrode and a Saturated Calomel Electrode Fe2+ ions concentration is reduced to 1/10 (0.003 M) of the original
(SCE, 241 mVSHE ) as the reference electrode. All potentials refer recipe. Our findings indicate that there is a threshold around pH
to the SCE. A potential pulse technique was used with an “on” 3.4 for gallium deposition using the given co-deposition electrolyte
deposition potential E1 and an “off” potential E2 that were applied system.
for t1 = t2 = 3.9 s. E1 is equivalent to the reduction peak voltage Only when the pH is 4.0 can a homogenous film be deposited
measured from cyclic voltammetry prior to each electroplating across a large area substrate with a length of a few centimetres.
experiment. E1 lies in the range between −2.05 V and −2.25 V. Due to the competitive nature between the Ga3+ and Fe2+ depo-
The “off” potential E2 was set at −0.9 V. The current during the sition mechanisms, any variations in the uniformity of either the
second step E2 was almost zero, which effectively enables the com- rate of diffusion of the chemical species arriving at the surface of
pensation of pH and concentration gradients of the metal ions. the substrate or of the current density across the substrate, would
All experiments were performed at room temperature without create variations in the Ga:Fe deposition ratio.
mechanical stirring. The copper foil was cleaned using isopropanol, As quantified by Element Dispersive X-Ray (EDX) elemental
acetone and deionised water. Before plating the foil was immersed analysis, a Ga0.19 Fe0.81 film was achieved for a pH of 4.0 and 0.006 M
in Procirc 921 micro-etch solution for 10 mins to remove the cop- Fe2+ concentration. This Ga:Fe ratio is close to that required for
per oxide surface layer. Oxygen from the electrolyte solution was optimal magnetostrictive behaviour [13]. Further reduction of the
purged by the nitrogen gas for 10 mins prior to experiments and Fe2+ to 0.003 M Fe2+ concentration resulted in the deposition of a
left blowing over the solution during the experiments. Ga0.29 Fe0.71 film. A separate EDX element mapping was carried out
According to a previously proposed deposition mechanism [4,5], on a cross-sectional view of the Ga0.29 Fe0.71 sample as shown in
each cycle led to Fe–Ga alloy deposition in parallel with gallium Fig. 2. The results obtained for Ga0.19 Fe0.81 were found to be similar
hydroxide precipitation during the forward potential application to those obtained for the Ga0.29 Fe0.71 sample. The preparation of
E1 and the re-dissolution of hydroxide during the reverse poten- the film was performed using Broadband Ion Beam (BIB) machin-
tial step E2 . A dense Fe–Ga alloy deposit with low oxygen content ing by the Company MCS Ltd [14], which allows deformation and
can only be achieved when hydroxide formation and re-dissolution smear-free cross-sectioning without obscuring the sample surface.
are eliminated. The refined electrolyte recipe, which used sodium The process uses a BIB system, which allows representative sam-
citrate as a complexing agent for the metal ions (Fe2+ , Ga3+ ), allowed ple sizes of up to 2 mm to be cross-sectioned without mechanically
a stable electrolyte to be operated at a less acidic level close to pH touching the sample. This is a significant step change, which enables
3.0 as opposed to pH 2.0 found in previous literature [10–12]. At this absolute confidence that deformation of the device did not occur
pH level, hydrogen evolution was significantly reduced. However, during preparation for analysis. The samples were analysed using
the increased stability of the Ga3+ ions also means that the release a combination of Field Emission Scanning Electron Microscopy
of Ga3+ ions became slower, especially when compared to the fast (FESEM) and EDX. The individual element maps of Ga and Fe indi-
rate of Fe electrodeposition in the co-deposition electrolyte system. cate no gradient in Ga content and that the Ga is evenly distributed
As a consequence, the resultant deposition contained prevalently within Fe–Ga alloy film. There is also no oxygen content detectable
Fe with almost no detectable trace of Ga. by the EDX, meaning that no gallium hydroxide was incorporated
To remedy this situation, Iselt et al [4,5]. increased the metal ion into the deposit during the electrochemical deposition. The cross-
ratio Ga3+ :Fe2+ to more than 2:1 in order to enhance the reactivity section of an oxygen-free, dense Ga0.29 Fe0.71 electrodeposited thin
 J.H.-G. Ng et al. / Sensors and Actuators A 223 (2015) 91–96 93

Fig. 2. EDX Ga, Fe and overlaid element maps on a cross-sectional overview.

film is imaged by the FESEM as shown in Fig. 3 (top image) and

found to have an average film thickness of approximately 600 nm
after 115 plating cycles. The interface between the alloy and the
substrate seems more interstitial as observed in Fig. 3 (bottom
image) in the case of a sample with only Fe electrodeposited from
the co-deposition electrolyte system.
FESEM images from the surface of the deposited film also indi-
cate that homogeneous deposition of the alloy took place as no
separate Ga and Fe aggregate domains can be observed for both
the Ga0.19 Fe0.81 and the Ga0.29 Fe0.71 samples as shown in Fig. 4.

3. Measurement of the magnetostrictive effect

A 20 ␮m thick copper foil was plated with a 1 ␮m thick

Ga0.19 Fe0.81 film at pH 4.0. Then the foil was used as a substrate
for cutting 5 mm long and 1 mm wide cantilevers, as those shown
in Fig. 5. The cutting process was performed using a frequency-
doubled diode-pumped Yb:YVO4 laser (Spectra Physics Lasers, Inc.)
which provided 65 ns pulses with a 30 kHz pulse repetition fre-
quency at a 532 nm wavelength. The cutting of cantilevers was
performed by moving a focused laser beam across the foil at a
20 mm s−1 velocity using a galvo-scanner, which was equipped
with a 108 mm focal length flat-field (T-theta) lens to provide an
approximately 16 ␮m diameter spot on the foil. The pulse energy
used for cutting was 130 ␮J corresponding to a 3.9 W average
power, whilst the cutting tolerance was better than ±20 ␮m.
A magnetostrictive material such as Galfenol always strains pos-
itively in a magnetic field irrespective of the field direction. If the
film is deposited on the top surface then the cantilever will bend
downwards in the presence of a parallel magnetic field. This was
found to be the case. Since the deflection was small compared to
the cantilever length and of the same magnitude irrespective the
parallel field direction the magnetostatic forces were assumed to Fig. 3. Cross-sectional FESEM images of top the electroplated Ga0.29 Fe0.71 alloy and
be negligible. bottom the electroplated Fe film with no detectable Ga.
94 J.H.-G. Ng et al. / Sensors and Actuators A 223 (2015) 91–96

Fig. 6. Experimental setup for the measurement of the deflection of the cantilever
beam.

Agilent 33220A pulse generator. The field between the pole faces
was measured by a Hirst flux probe, located between the pole faces
and labelled B.

3.2. Modelling of the strain in the Galfenol film

Fig. 4. Top view FESEM images of (a) Ga0.19 Fe0.81 and (b) Ga0.29 Fe0.71 electrode- The cantilevers are modelled as a beam with one simply sup-
posited films. ported end and the other end free. The beam is constructed of two
materials of different Young’s modulus and thickness as shown in
Fig. 7. The strain in the Galfenol film, , can be calculated using Eq.
3.1. Test setup
(1) [5]:
A C-core used power transformer, Wiltan type 10/8/13, was (1 + vg ) · (ECu · t 2 ) · D
machined to produce a 15 mm gap between the pole faces [15]. = (1)
3L2 · Eg · d · (1 − vCu )
Eighty-eight turns of 1 mm2 copper wire was wound on the core
to provide up to 60 kA/m between the pole faces. The experi- where Eg and ECu are the Young’s moduli of Galfenol and copper,
mental setup is shown in Fig. 6. Vertical deflection was measured respectively and t is the thickness of substrate, here the copper
using a Micro Epsilon NCDT2400 confocal displacement probe foil. D is the deflection of the beam, d is the Galfenol film thickness
[16], denoted by the label A in the figure. The field intensity was and g and Cu are the Poisson’s ratios of Galfenol film and copper,
measured at the cantilever end. The output was averaged over respectively. L is the length of the cantilever. The values of Eg were
5 measurements and sampled at 300 Hz, which enabled the dis- taken from [4] and values of ECu and Cu were taken from [5].
placement to be measured within ±50 nm. Background vibrations
were minimised by bolting the rig to a Newport mini optical 3.3. Experimental results
table. Current was switched using a type 20N06 MOSFET via and
With the beams mounted in the test jig shown in Fig. 7, pulse
fields were applied onto the cantilevers with the confocal probe
focused on each beam in turn. Fig. 8 shows a typical deflection

Nylon clamp B
FeGa

L Cu

Fig. 7. Schematic of the cantilever of length L. B is the applied field with the arrows
indicating direction. FeGa is the Galfenol film. In this configuration the deflection D
Fig. 5. Optical microscope image of the laser cut cantilevers. is always downwards if the film is magnetostrictive.
 J.H.-G. Ng et al. / Sensors and Actuators A 223 (2015) 91–96 95

1.2 developed that enables the deposition of solid and consistent films
1 close to the ideal composition of 80:20 iron/gallium concentration
Deflection (μm)

0.8
with high tolerance towards current density variations, making
0.6
0.4
it ideal for the electrodeposition of micropatterned structures
0.2 for MEMS devices. A first potential magnetostrictive applica-
0 tion is demonstrated in the form of bilayer cantilever beams
-0.2 0 10 20 30 40 50 that deflect in response to an external bias magnetic field. A
-0.4 600 nm thick Ga–Fe alloy film was grown on top of a 20 ␮m
-0.6
Time (s) thick copper foil after 115 plating cycles and subsequently cut
to form millimetre-size cantilever beams. The deflection of the
Fig. 8. Beam deflection in ␮m as a function of time with a 40 mT (31 kA/m) applied beams in response to an external magnetic excitation supplied
field with duty cycle of 50%. by a custom-built test rig was monitored. A strain coefficient
at maximum deflection was measured to be  = 96 ppm The
observed magnetostrictive properties represent a promising result
1.4 for further application into more complex MEMS and millime-
1.2 tre scale devices such as magnetic field sensors or magnetic
Deflection (μm)

1 actuators.

0.8

0.6

0.4 Acknowledgment
0.2
The authors acknowledge the funding from the British Engineer-
0
-60 -50 -40 -30 -20 -10 0 10 20 30 40 50 60 ing and Physical Research Council (EPSRC) under the Innovative
Field Strength (kAm-1) electronic Manufacturing Research Centre (IeMRC) through its flag-
ship project “Smart Microsystems” referenced FS/01/02/10.

Fig. 9. Deflection in microns of the cantilever beams as a function of the field

strength for Fe0.81 Ga0.19 and Fe0.71 Ga0.29 samples. The vertical error bars at ±1
standard deviation are about 50 nm. References

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96 J.H.-G. Ng et al. / Sensors and Actuators A 223 (2015) 91–96

Biographies
Giuseppe Schiavone received the B.Eng. degree in phys-
ical engineering and the M.Sc. degree in micro and
nanotechnologies from Politecnico di Torino, Italy, in 2007
Jack H.-G Ng graduated from Heriot-Watt University and 2009, an M.Sc. degree in micro and nanoelectronics
with a Ph.D. in simplifying metals fabrication for micro- from Univérsité Joseph Fourier, Grenoble, France, in 2009,
engineering and is the first inventor of a patent of an and the Ph.D. degree in magnetic MEMS from the School of
artificial photosynthesis-inspired manufacturing process. Engineering of the University of Edinburgh, U.K., in 2014.
Following his further post-doctorate positions in fabrica- He is currently a Research Associate with the Research
tion and packaging of sensors at the applied chemistry Institute of Signals, Sensors and Systems in the School of
level, he has been awarded by The Royal Society of Edin- Engineering & Physical Sciences at Heriot-Watt Univer-
burgh and Scottish Enterprise as an Enterprise Fellow sity.
currently commercialising the antimicrobial property of
copper in order to reduce infections in the healthcare envi- Eitan Abraham was born in Israel, obtained his first
ronment. degree from the University of Buenos Aires, and his
Ph.D. from the University of Manchester. He is a the-
Paul M. Record graduated from Strathclyde University oretical physicist and Associate Professor of Physics at
with a Ph.D. and has worked on biomedical instrumen- Heriot-Watt University. He is and presently a mem-
tation for visual prosthesis at University of Birmingham ber of the Institute of Biological Chemistry, Biophysics
and electrical impedance imaging at University of Keele. and Bioengineering. His new research interests are bio-
Later work included instrumentation for satellite relay physics and quantum physics. In the 1980s he pioneered
data loggers for phocids and cetaceans in the open ocean ideas in optical computing and has worked in nonlin-
at University of St. Andrews. Work on implanted RF linked ear optics, nonlinear dynamics of optical and Josephson
tags for these animals lead to an interest in RFIDs and junction systems and superconductivity. Together with
embedded antennas in the 10 MHz to 2 GHz bands. Cou- Prof Desmulliez he started the company MicroStencil Ltd
pled work on sensors included magnetostrictive materials specialised in electroformed stencils for microelectronics
for wireless sensors. He has three patents on antennas, applications.
electric field sensors and tag synchronisation.
Gerard Cummins received his B.Eng. degree in electrical
Xinxin Shang graduated from Heriot-Watt University in and microelectronic engineering from University College
2013 with an M.Sc. degree in materials for sustainable and Cork, Ireland in 2003 and his Ph.D. degree in microengi-
renewable energies. neering from the School of Engineering of the University of
Edinburgh, U.K. in 2011. He is currently a Research Asso-
ciate with the Institute of Signals, Sensors and Systems in
the School of Engineering and Physical Sciences at Heriot-
Watt University.

Krystian L. Wlodarczyk graduated from the Wroclaw Marc P.Y. Desmulliez graduated from the Ecole
University of Technology (Poland) in 2006 with an M.Sc. Superieure d’Electricite of Paris, Paris, France, in 1987.
degree in electronics and telecommunications. Then, he He received two College Diplomas in microwave and
joined the Lasers and Photonics Applications group at modern optics from University College London, London,
Heriot-Watt University as a PhD student. Krystian’s Ph.D. U.K. and in theoretical physics from the University of
research studies involved CO2 laser micro-machining of Cambridge, Cambridge, U.K., in 1987 and 1989 respec-
optical glasses and investigating new applications for CO2 tively. He received the Ph.D. degree in optoelectronics
laser polishing. He graduated with a Ph.D. degree in June from Heriot-Watt University, Edinburgh, U.K., in 1995.
2011. Currently, Krystian is a Research Associate within He is currently The Head of the Research Institute of
the High Power Laser Application group at Heriot-Watt Signals, Sensors and Systems in the School of Engineering
University where he works on various projects involving & Physical Sciences at Heriot-Watt University, and has
laser processing of metals and optical glasses. been directing the Microsystems Engineering Centre
since 1999.

Duncan P. Hand has been a member of staff at Heriot-

Watt University for over 20 years, following a PhD in
fibre optics at the University of Southampton. The focus
of his research activity is applications of high power
lasers, in particular in manufacturing, and he is Direc-
tor of the EPSRC Centre for Innovative Manufacturing in
Laser-based Production Processes, a 5-university Centre.
Other research focuses on delivery of high peak power
laser light through novel microstructured optical fibres
(with Bath University), with applications in manufactur-
ing and medicine. He is also currently Director of Research
and Deputy Head of the School of Engineering and Physical
Sciences.