IEEE TRANSACTIONS ON ELECTRONICS PACKAGING MANUFACTURING, VOL. 32, NO.

4, OCTOBER 2009 265

Cross-Section Preparation for Solder Joints and

MEMS Device Using Argon Ion Beam Milling
Omid Mokhtari Amirmajdi, Roya Ashyer-Soltani, Michael Paul Clode, Samjid H. Mannan, Senior Member, IEEE,
Yunqi Wang, Enric Cabruja, and Giulio Pellegrini

Abstract—Mechanical cross-section polishing has traditionally

been the method of choice for preparing samples to be examined
by Scanning Electron Microscopy (SEM). Although mechanical
polishing, allied to selective chemical etching can reveal the most
important characteristics of solder joint microstructure, subtle
details may be lost. A relatively new cross section polishing method
has been developed using an Argon ion beam to prepare a flat sur-
face with potentially less sample damage. In this study we compare
these two methods of cross section polishing for solder-substrate
couples, and for delicate MEMS type structures. Four solder
samples were prepared, consisting of SAC (Sn-Ag-Cu) solder, SAC
Fig. 1. Schematic of CSP operation for cross-section preparation.
solder on copper substrate, SAC solder on nickel substrate and
In-Sn solder on niobium substrate. SEM was used to examine
the polished samples and it was found that features such as the
internal structure of intermetallic compounds (IMCs) was more cracks, and samples containing both very hard and very soft
readily identified using the new technique. The ion beam milling constituents. The abrasive particles (e.g., silicon carbide or di-
technique was also found to be more suitable for simultaneous
amond) can also become embedded in any soft phases present.
observation of multiple aspects of microstructure (e.g., identifi-
cation of IMCs in relation to grain boundaries, substrate crystal In order to overcome these problems, a new polishing method
structure or the eutectic solder structure). The MEMS device and equipment based on the use of a beam of argon ions directed
cross-sections could only be prepared by the ion beam method as at the sample has been developed by Jeol, Ltd. [1]–[3], and the
mechanical polishing caused too much damage. utility of this method for electronics packages and structures ex-
Index Terms—Cross-section polisher, lead-free, Sn–Ag–Cu, amined in this paper.
solder. Improved methods of microstructural investigation are of
interest particularly as miniaturization of solder joints, in-
creased use of electronics in high-temperature environments
I. INTRODUCTION
and the introduction of Pb-free solders produces new solder
joint microstructures. Variants of Sn–Ag–Cu (SAC) alloys

M ECHANICAL grinding and polishing has been used for

scanning electron microscopy (SEM) sample prepara-
tion due to ease of preparation and low cost of use. The basic
principle is that successively finer grades of abrasive powders on
rotary polishing cloths are used to produce extremely flat, high-
quality samples. A lubricant is also used to minimize sample
damage. However, this method can distort delicate structures
such as thin membranes, and also samples containing voids,
Manuscript received January 30, 2009; revised June 29, 2009. Current version
published October 07, 2009. This work was supported by IeMRC under Grant
SP/06/03/01. This work was recommended for publication by Associate Editor
A. Shapiro upon evaluation of the reviewers comments.
O. Mokhtari Amirmajdi, R. Ashyer-Soltani, M. P. Clode, and S. H.
Mannan are with the Department of Mechanical Engineering, King’s Col-
lege London, London WC2R 2LS, U.K. (e-mail: omid.mokhtari@kcl.ac.uk;
omid.mokhtari@gmail.com; roya.ashayer@kcl.ac.uk; mike.clode@kcl.ac.uk;
samjid.mannan@kcl.ac.uk).
Y. Wang is with the Department of Physics and Materials Science, City Uni-
versity of Hong Kong, Kowloon, Hong Kong SAR (e-mail: 50728132@student.
cityu.edu.hk).
E. Cabruja and G. Pellegrini are with IMB-CNM (CSIC), 08193 Bellaterra,
Spain (e-mail: enric.cabruja@cnm.es; giulio.pellegrini@cnm.es).
Color versions of one or more of the figures in this paper are available online
at http://ieeexplore.ieee.org.
Digital Object Identifier 10.1109/TEPM.2009.2029344
1521-334X/$26.00 © 2009 IEEE
are the most likely candidate for Sn–Pb solders replacement
[4]. The three phases which are in equilibrium in SAC alloy
are Sn, Ag Sn, and Cu Sn [5]. Precise understanding of
the relationships between these phases and the intermetallic
compounds (IMCs)s formed after reaction with the substrate
are required for reliability predictions. Similarly, the growing
use of microelectromechanical systems (MEMS) requires
new sample preparation methods as mechanical polishing can
shatter structures made of brittle materials such as Si.
The equipment used for argon ion beam milling in this study
is the JEOL SM-09010 Cross Section Polisher (CSP). An argon
ion beam is produced and directed towards the sample and shield
plate to mill the unshielded part of the sample. This results in a
sample cross section that is of the order of 1 mm in width and
which is produced perpendicular to the plane of the shield plate
as shown in Fig. 1. Targeting of particular features by aligning
them against the shield is possible with the aid of a loupe to an
accuracy of approximately 10 m. Because of the near-zero in-
cident angle of the ion beam, the quantity of implanted ions into
the cross-section region is very small and deposition of the ele-
ments from the shield plate is also minimized [1]. Furthermore,
since the specimen is in intimate contact with the metal shield
plate and mounting block, temperature rises during milling will
266 IEEE TRANSACTIONS ON ELECTRONICS PACKAGING MANUFACTURING, VOL. 32, NO. 4, OCTOBER 2009
Fig. 2. Schematic of CSP operation for etching.
be minimized. Focused ion beam (FIB) milling is a similar tech-
nique, but the size of the polished surface is of the order of tens
of square micrometers. Thus, FIB is applicable only when long
preparation times are acceptable [1], [6].
The argon ion beam also provides an excellent method of
etching in order to increase the contrast between phases, in a
similar way to chemical etching with dilute acid. In order to
achieve this, the shield plate was removed and the mounting
block rotated through 90 , as shown in Fig. 2.
II. SAMPLE PREPARATION
A. Solder Sample Preparation
The lead-free solder paste Sn–3.8Ag–0.7Cu (SAC) samples
were prepared on Cu substrate, Electroless Ni Immersion Gold
(ENIG), and inert (glass) substrates. For observation on the inert
substrate, a small amount of solder paste was placed on a mi-
croscope slide which was then placed inside a bench-top oven
(MRO 160). The paste was preheated for 150 s at 140 C and
soldered for 60 s at 260 C. Immediately after the soldering
stage, while the solder was molten, a heated metal weight (also
placed inside the oven during the reflow) was placed on the
solder to reduce the solder thickness down to 0.410 mm (thick-
ness controlled by spacers). Although the CSP can accommo-
date samples up to 2 mm thick, thinner samples reduced the
preparation time.
For the SAC solder on Cu substrates, cm cm
mm copper foils were used. SAC solder paste weighing
0.05g was placed on the Cu foil supported by a glass side and
reflowed using the method described above. ENIG pads were
used for the SAC solder on Ni substrates. The metal pad and
top layers of the printed circuit board (PCB) were peeled off
the glass fibre reinforced PCB, leaving a substrate thickness of
0.25 mm. SAC solder was printed through a 0.2-mm stencil onto
the pad and again the same reflow profile and thinning method
was used, resulting in a 0.65-mm-thick sample.
Cross sections of these samples were prepared using the CSP
and mechanical polishing. For the CSP, the samples were at-
tached onto the mounting block using a thin layer of wax heated
to 100 C. The block was then positioned with the sample jutting
out approximately 50 m from the shield plate (see Fig. 1) and
the milling chamber was filled with low pressure Ar gas. The
accelerating voltage (typically 5.0–5.5 kV) of the ion beam and
Fig. 3. Schematic view showing the new detector concept.
milling time (typically 24–35 h) were set and the CSP was al-
lowed to operate without further intervention. Further details on
the operation of the CSP can be found in [1]. After the cross sec-
tions were formed, the samples were etched as shown in Fig. 2,
using 4 kV for 30s.
Mechanically polished samples were soldered following
the same procedure as the CSP samples (including the use of
a weight to reduce sample thickness). They were then cold
mounted in a standard epoxy potting compound. The mounted
SAC samples were then polished using P240-, P600-, and
P1200- grit silicon carbide papers. Next, the samples were pol-
ished using diamond suspensions of 3 m and finally 0.25 m.
Finally, the cross sections were etched in a solution of 2% nitric
acid in water for 10 s.
Solder joints formed of eutectic 52In–48Sn solder on Nb sub-
strate joining IGBT components to an alumina base have previ-
ously been prepared, and are described in detail elsewhere [7].
The assemblies were thermally cycled as described in [7] before
mechanical polishing using the same procedure as for the SAC
solder. Cross sections prepared using the CSP were made by
first cutting the assemblies with a diamond saw, potting the sam-
ples, and grinding back to a thickness of approximately 1 mm.
The samples were then mounted and cross sectioned by the CSP
using the same procedure as the SAC solders.
B. MEMS-Type Device Preparation
The analyzed device is a radiation detector with a thin perfo-
rated membrane; see Fig. 3 [8]. The main step in the realization
of ultra thin 3-D silicon detector is to combine the technology
for the fabrication of standard 3-D detectors with the thinning of
planar devices. A process to produce high-aspect-ratio holes in
the substrate using a combination of micromachining and stan-
dard planar fabrication technology was developed. In this case,
the main achievement was to control the process which must
stop at the SOI oxide interface, avoiding notching at the bottom
of the electrode. These holes were etched with an inductively
coupled plasma (ICP) device in the clean room facility at the
CNM-IMB in Barcelona. Various hole diameters are being in-
vestigated although for this fabrication run we used only 5 m.
Fig. 3 shows a cross section of a hole filled with polysilicon, the
diameter of the hole is 5 m and the depth is 10 m.
MOKHTARI AMIRMAJDI et al.: CROSS-SECTION PREPARATION FOR SOLDER JOINTS AND MEMS DEVICE USING ARGON ION BEAM MILLING 267

Fig. 4. Views of MEMS device. (a) Overview of MEMS device membrane. (b) Close-up of via in pad.

Fig. 5. SEM cross-sectional views of SAC bulk. (a) SAC solder sample was polished and etched using CSP. (b) SAC solder sample was mechanically polished
and chemically etched.

Two sets of holes must be etched separately and then filled
with polysilicon doped with boron and phosphorus to form a
p-n junction. After the first set of holes is filled with polysilicon
and then doped, a thin layer of thermal oxide is grown on the
surface in order to protect these holes from the following etching
and polysilicon deposition and doping. The polysilicon is then
patterned on the surface and left only around the hole openings
in order to ensure the contact with the aluminum. The wafers
are then passivated with silicon nitride for protection.
The final step is the thinning of the back surface of the active
detector area. This results in a membrane which has been cross
sectioned and analyzed. The thinning is done using a TMH so-
lution which stops the etching at the oxide interface of the SOI
wafer. The oxide layer is then etched away.
In contrast to the solder samples, the cross section of the
MEMS device needed to include a specific feature; the 5- m-di-
ameter vias located on the pads on the chip. Devices were sec-
tioned using a diamond saw and also using a scalpel. In both
cases, significant damage was done to the thin Si membrane, but
although the sample edges were damaged, pads lying 20–30 m
from the edge were undamaged. A portion of the thin Si mem-
brane was mounted with wax onto the mounting block. The
mounted specimen was aligned with a row of pads approxi-
mately parallel to the shield plate (a small relative angle of
1 –2 was maintained in order to maximize the chance of cut-
ting through the middle of at least one via on the row). The beam
conditions were set to 5 kV for 10 h and vias were found at the
first attempt.
In order to obtain mechanically polished samples, the devices
were sent to an electronics packaging analysis lab with con-
siderable expertise in mechanical polishing techniques. How-
ever, after potting and mechanical polishing, it was found im-
possible to cross section the 10- m-thick Si membranes due to
their brittle nature.
III. EXPERIMENTAL RESULTS AND DISCUSSION
A. MEMS Cross Sections Prepared With CSP
The MEMS cross sections are of particular interest because
only the CSP was able to produce suitable cross sections. The
SEM used to take images was the FEI Quanta 200 FEG. Element
analysis was carried out with an EDAX spectrometer. All the
images in this paper have been taken by SEM in back-scattered
mode except Fig. 11(b) which has been taken in secondary elec-
tron mode. Consequently, the contrast is generally generated by
atomic number (Z) of the materials present. The accelerating
voltages in all images are 10.0 kV except for Figs. 4 and 5(b)
for which the voltages are 20.0 kV and 25.00 kV, respectively.
268 IEEE TRANSACTIONS ON ELECTRONICS PACKAGING MANUFACTURING, VOL. 32, NO. 4, OCTOBER 2009
Fig. 6. SEM cross-sectional views of IMC in SAC on Cu substrate. (a) SAC on Cu substrate polished and etched by ion beam miller. (b) SAC on Cu substrate
polished mechanically and chemically etched.
Fig. 7. SEM cross-sectional views of IMC in SAC on Ni substrate. (a) SAC on Ni substrate polished and etched by ion beam miller (b) SAC on Ni substrate
polished by mechanical polishing and etched chemically.
Fig. 4(a) shows a cross section of the Si membrane together
with an overview of the pad and via layout on the device.
Fig. 4(b) shows a close-up of the pad and via.
In the cross section, we can distinguish the P-N junction
around the vias. This has been electrically confirmed after the
test. In addition, one can see the homogeneity in the deposition
of the filling polysilicon all along the via depth.
B. CSP Versus Mechanical Polishing
In order to compare mechanically polished and CSP images,
the same magnification and voltage settings were used for each
pair of mechanically polished and CSP prepared samples. Fig. 5
presents images of the bulk solder samples (solder on inert sub-
strate). Although these are taken from different areas, both are
representative examples of the bulk microstructure. While both
methods show the IMC structures in detail, only the CSP pre-
pared image simultaneously shows details of the Sn phase as
the etching has removed details of this phase from the mechan-
ically polished sample. Additional high-quality images of bulk
SAC solders may be found in, e.g., [9] and [10], but the same
conclusion may be drawn.
Comparison of the SAC on Cu samples is shown in Fig. 6(a)
(CSP) and 6(b) (mechanically polished). There appears to be a
large difference in size between the two samples even though
they were prepared under identical conditions. The discrepancy
may be caused by the fact that for sample 6(a) the cross sec-
tion was taken 75 m from the edge of the substrate while for
6(b), the grinding and polishing operations resulted in a section
further in towards the center. It is also clear that the mechanical
polishing resulted in scratches and embedded particles (both Sil-
icon carbide and diamond) which might be less pronounced with
expert polishing. However, both the CSP and mechanical pol-
ishing were undertaken by relatively inexperienced researchers,
and it was of interest to test the claims of the CSP manufacturer
that high quality surfaces can be produced with the CSP without
expert knowledge.
Fig. 6 also shows that the CSP method was able to simul-
taneously define the crystalline structure of the Cu substrate,
both the Sn and Ag Sn phases in the solder while the me-
chanically polished sample was unable to show details of the Cu
substrate or the bulk solder. Although the CSP method shows a
Cu Sn IMC layer that is not present in the mechanically pol-
ished sample, this may be due to the smaller IMC layers present
in the latter. Superior quality mechanically polished samples of
SAC on solder can be viewed in refs. [9], [11], [12], but the
general point that the CSP is able to image more aspects of the
microstructure than mechanical polishing remains valid.
Next we examine SAC on Ni samples in Fig. 7. Again, the
limitation of the CSP only being able to image samples 75 mi-
crons from the edge of the sample is apparent as the solder is
MOKHTARI AMIRMAJDI et al.: CROSS-SECTION PREPARATION FOR SOLDER JOINTS AND MEMS DEVICE USING ARGON ION BEAM MILLING 269

Fig. 8. Images at the 52In-48Sn/Nb interface. (a) prepared using CSP. (b) prepared by mechanical polishing method [7].

Fig. 9. Image at the 52In-48Sn/Nb interface. (a) prepared using CSP. (b) related system with larger IMC crystals prepared by mechanical polishing [13].

only a few microns thick at the edge of the pad [Fig. 7(a)].
This results in a markedly different microstructure from the me-
chanically polished sample sectioned through the middle of the
pad [Fig. 7(b)]. Of course, the sample could first have been cut
through the middle of a pad with a diamond saw, but the saw
might induce cracks or other features artificially. One way of
avoiding this problem might be to mill away 75 micron slices of
the sample sequentially but this would be time consuming. An
additional artefact induced by the CSP were the vertical stria-
tions caused by the ion beam. These can be eliminated by in-
creasing beam voltage and decreasing milling time.
Finally in this section, we compare the In-Sn/Nb samples.
Mechanical polishing of these samples has proven consistently
problematic because of the presence of the extremely soft In-Sn Fig. 10. Bulk SAC solder prepared by CSP showing detail of primary Ag Sn.
solder in proximity to an extremely hard refractory metal Nb
layer. Fig. 8(a) shows the CSP sample, and includes detail of
both the Nb layer, the IMC layer (composed of platelets higher temperatures in order to grow the IMC layer. It is still
that extend into the solder) and the solder. By contrast, the me- noticeable that the CSP image reveals additional details such as
chanically polished sample in Fig. 8(b) show only the Nb layer the orientation of the IMC crystals with respect to the under-
in detail and the solder has not been sufficiently well polished to lying Nb crystals. Although the IMC structure in Fig. 8(a) is
show up the IMC crystals. Fig. 9(a)) shows a lower magnifica- superficially similar to the polishing artefacts of Fig. 7(a) (ion
tion image of the CSP sample while Fig. 9(b)) shows a related beam parallel to the artefacts), it should be noted that the direc-
system (Fig. 7(c) in [13]) which has been aged longer and at tion of the ion beam was at right angles to the IMC structures in
270 IEEE TRANSACTIONS ON ELECTRONICS PACKAGING MANUFACTURING, VOL. 32, NO. 4, OCTOBER 2009
Fig. 11. Large Ag Sn plate in SAC on Cu sample prepared by CSP and high magnification of inset in (b).
Fig. 12. Bright Ag3Sn and darker Cu6Sn5 IMCs dispersed in SAC solder.
Fig. 8(a) and so could not have been caused by the same mech-
anism.
C. Details of SAC Solder Morphology Revealed With CSP
In this section we focus on details of the SAC solder which
are revealed with the CSP and which are not generally observed
with mechanical polishing. The CSP method reveals variations
in composition inside IMC structures as shown in Fig. 10 where
it can be seen that the core of the Ag Sn IMCs contains dark
spots which were found to have depleted levels of Ag. Fig. 11.
shows a large Ag Sn plate IMC with detailed internal platelet-
like structures. Fig. 12 shows primary Ag Sn and Cu Sn IMCs
dispersed within bulk SAC solder and reveals that each Cu Sn
crystal is in contact with a Ag Sn crystal.
While grain boundaries in SAC solders can be observed
using optical microscopy, or revealed using selective chemical
etching, the CSP method reveals both grain boundaries and
IMC location automatically. Fig. 13 reveals a Cu Sn IMC at
the intersection of three Sn grains.
Fig. 13. Backscattered cross-sectional image of bulk SAC (from SAC on Ni
sample).
IV. CONCLUSION
While mechanical polishing remains the quickest and
cheapest method of obtaining cross sections suitable for SEM
imaging, the CSP has benefits in a number of scenarios. First,
when the sample is composed of delicate or brittle structures,
mechanical polishing may not be an option. Second, the CSP is
superior over mechanical polishing when the system contains
structures encompassing a large range of hardness. Third, in
the absence of expert knowledge of mechanical polishing tech-
niques, the CSP is able to reveal greater details about a range
of structures within the system than is possible using simple
mechanical polishing and etching. A practitioner using CSP
requires only a basic level of familiarity with the instrument
to produce samples similar in quality to those produced by an
expert in the techniques of mechanical polishing. The third
benefit will be of particular value for failure analysis when the
nature of the problem will not a priori be known. Certainly
more specialized techniques such as TEM or FIB could be used
to focus on individual features, but the CSP is able to deliver
a detailed overview.
MOKHTARI AMIRMAJDI et al.: CROSS-SECTION PREPARATION FOR SOLDER JOINTS AND MEMS DEVICE USING ARGON ION BEAM MILLING
ACKNOWLEDGMENT
The authors would like to thank Dr. A. Brain for his help in
taking the SEM images.
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Omid Mokhtari Amirmajdi received the
B.Sc.(Eng.) degree in mechanical engineering
from Azad University of Mashhad, Mashhad,
Iran, in 2006 and the M.Sc. degree in innovation,
commercialization, and entrepreneurship from the
University of Stirling, Stirling, U.K., in 2007. He is
currently pursuing the Ph.D. degree in the Division
of Engineering, King’s College London, London,
U.K., where his field of research is on nanoparticle
enhanced solders for increased solder reliability.
Roya Ashyer-Soltani received the B.Eng. degree
(honors) in chemical engineering and the Ph.D.
degree in a petroleum-related subject from Imperial
College, London, London, U.K.
She is currently with the Department of Mechan-
ical Engineering, Kings College London, and her re-
search is based on the synthesis of nanoparticles and
their implementation in solder.
View publication stats
271
Michael Paul Clode received the B.Sc. degree in
mechanical engineering and the Ph.D. degree in
mechanical metallurgy from Imperial College of
London, London, U.K., in 1983 and 1987, respec-
tively.
In 1989, Michael was appointed Lecturer in
Metallurgy in the Department of Mechanical
Engineering at King’s College London, where his
research interests continued in the field of nonferrous
materials and manufacturing processes, including
the metallurgy and mechanical properties of novel,
high-performance solders.
Dr. Clode is also a Fellow of the IoM3.
Samjid H. Mannan (SM’07) received the B.A.
degree in physics from Oxford University, Oxford,
U.K., in 1988 and the Ph.D. degree in physics from
Southampton University, Southampton, U.K., in
1991.
He worked in the area of electronics packaging at
Salford University, Salford, U.K., and Loughborough
University, Leicestershire, U.K., until 1999, when
he joined King’s College London, London, U.K. He
was appointed Reader in Electronics Manufacturing
in 2007. His current interests include rheology of
dense suspensions (e.g., solder paste) and packaging for high-temperature
electronics, including nano-composite solders.
Yunqi Wang received the B.Sc. degree in materials
engineering from the City University of Hong Kong
(CityU of HK) in 2009.
She participated in research on lithium batteries at
CityU of HK as a Research Assistant and finished the
graduation dissertation on ZnO nanowire solar cells
under the supervision of Prof. Igor Bello. In 2008, she
conducted an internship project on soldering super-
vised by Dr. S. Mannan at King’s College London.
Enric Cabruja received the Ph.D. degree in physics
from the Universitat Autònoma de Barcelona,
Barcelona, Spain.
He has been a Tenured Scientist since 1993 at
the Spanish Council for Scientific Research (CSIC).
He is currently with the National Microelectronics
Center (CNM), Barcelona. He is responsible for
multichip modules and high-density packaging tech-
nologies. His main interests are high I/O bumping
and flip chip for particle detector applications.
Giulio Pellegrini received the Ph.D. degree in
physics from the University of Glasgow, Glasgow,
U.K.
He is currently with IMB-CNM-CSIC, Barcelona,
Spain. His main research focus is the development
and optimization of microelectronic technologies
for radiation detectors for their use in high-energy
physics, medical imaging, neutron dosimetry, and
space applications. He has also been working for
the collaboration ATLAS-SCT which aims to the
construction of a semiconductor tracker for CERN.