548 IEEE TRANSACTIONS ON COMPONENTS, PACKAGING AND MANUFACTURING TECHNOLOGY, VOL. 2, NO.
4, APRIL 2012
Low-Temperature and Pressureless Ag–Ag Direct
Bonding for Light Emitting Diode Die-Attachment
Masafumi Kuramoto, Teppei Kunimune, Satoru Ogawa, Miki Niwa, Keun-Soo Kim, and Katsuaki Suganuma
Abstract— Micrometer-sized Ag particles adsorb substantial
oxygen above 200 °C. A dispersion of these particles in alcohol
can be successfully used as a die-attach material by sintering the
Ag particles to form a soft porous bonding layer. Since the low-
temperature sintering of micrometer-sized Ag particles is unlikely
to involve the nanometer size effect associated with melting, it was
considered that the low-temperature sintering between Ag layers
of micrometer thickness would occur in air. The contact surface of
a light emitting diode die and a glass substrate were both coated
with an Ag sputtered layer of 2 µm in thickness. The Ag–Ag
direct bonding proceeded by sintering above 200 °C in air. The
bonding strength of the Ag–Ag direct bonding exceeded that of
the low-temperature sintering of micrometer-sized Ag particles,
and the bonding strength depended on oxygen concentration in
the sintering atmosphere. On the Ag sputtered surface of the
glass substrate, a substantial morphology change was observed
by heating the Ag sputtered layer in air. It was supposed that this
morphology change was caused by abnormal grain growth of Ag
in the Ag sputtered surface. It is concluded that low-temperature
sintering of Ag materials is accelerated by the abnormal grain
growth of Ag with oxygen adsorption near the Ag surface.
Index Terms— Die bonding, light-emitting diode, pressureless,
silver, sintering.
I. I NTRODUCTION
A S THE applications of power semiconductors have
continuously increased, suitable substitutes for high-
temperature high-lead solders are required. Lead-free materials
are needed to minimize the environmental impact of not only
electronic components but also assembled electronic appli-
cations. Die-attach materials for semiconductors that require
high-temperature driving conditions must also be lead-free for
added value. Light emitting semiconductors such as light-
emitting diodes (LEDs) and laser diodes are two such tar-
gets. Die-attach materials of power LEDs and laser diodes
Manuscript received April 25, 2011; revised July 28, 2011; accepted
December 5, 2011. Date of publication January 23, 2012; date of current
version March 30, 2012. This work was supported in part by a grant from the The p- and n- pad electrodes were then formed on the
NEDO Project Research and Development of alternatives to high-temperature
high lead solder operated by JEITA. Recommended for publication by
Associate Editor J. J. Liu upon evaluation of reviewers’ comments.
M. Kuramoto, T. Kunimune, and S. Ogawa are with the LED The luminescence peak wavelength of the LED die was then
Engineering Division, Nichia Corporation, Anan 774-0001, Japan
(e-mail: masafumi.kuramoto@nichia.co.jp; satoru.ogawa@tatsumi.nichia.co.jp;
teppei.kunimune@nichia.co.jp).
M. Niwa is with the Department of Intelligent Structures and Materials
Systems, University of Tokushima, Tokushima 770-8041, Japan (e-mail:
niwa@opt.tokushima-u.ac.jp).
K.-S. Kim and K. Suganuma are with the Institute of Scientific and
Industrial Research, Osaka University, Osaka 577-8502, Japan (e-mail:
kskim12@sanken.osaka-u.ac.jp; suganuma@sanken.osaka-u.ac.jp).
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/TCPMT.2011.2180385
2156–3950/$31.00 © 2012 IEEE
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must cause minimal disruption to the luminous efficiency.
The requirement to develop die-attach materials for power
LEDs is especially large because LEDs are expected to be
the next generation of light source, replacing conventional
lighting equipment such as fluorescent lamps and incandescent
lighting. The essential requirements for die-attach materials
are low thermal resistance, good thermal conductivity, good
reflectance, good resistance to heat degradation, and low-
temperature processability during assembly.
Ag is one of the best metals for optical applications due
in part to its high electric and thermal conductivities. It is
well known that Ag nanoparticles can be easily sintered at
low-temperature. Several reports detail the bonding process
using Ag nanoparticles [1]–[6]. One of the drawbacks asso-
ciated with using Ag nanoparticles is high cost. The authors
have found that micrometer-sized Ag particles adsorb oxygen
significantly above 200 °C, resulting in the formation of a
porous bonding layer structure upon sintering. It was also
found that the die-attach properties were superior [7], [8].
The proposition of a new LED die-bonding process that is
superior in electric resistivity, heat dissipation, and extraction
efficiency of light emitting semiconductors was investigated.,
The direct-bonding by low-temperature sintering between Ag
thin sputtered layers, the essential low-temperature sintering
mechanism of Ag particles, as well as the Ag sputtered layer,
were all clarified by the observation of a bonding interface
and morphology changes of the Ag sputtered surface.
II. E XPERIMENT
A. Sample Preparation
The external dimensions of the LED die were 600×600 µm
with a thickness of 80 µm. The LED die was formed by
deposition of a semiconductor layer containing InGaN on a
sapphire substrate by metal-organic chemical vapor deposition.
semiconductor layer. The bottom face of the sapphire substrate
was coated with an Ag layer having a thickness of 2.0 µm.
measured using a multi-channel photodetector. The lumines-
cence peak appeared at 460 nm, corresponding to a blue LED.
The die mounting substrate was found to have the following
structures. A Ti seed layer of 0.035-µm thickness was formed
on a glass slide (AS ONE Corporation, Osaka, Japan) using a
sputter method and a subsequent Ag sputtered layer of 2.0-µm
thickness was formed on the slide glass. The Ti layer was
needed to form a stable interface between the Ag layer and
the slide glass.
KURAMOTO et al.: LOW-TEMPERATURE AND PRESSURELESS Ag–Ag DIRECT BONDING
(a) (b)
Fig. 1. Scanning electron microscopy (SEM) images of (a) AgC239 and
(b) FHD. Both images are collected at the same magnification (×10 000).
p-pad electrode n-pad electrode
Ag 2 μm thickness
Ag 2-μm
80 μm Sapphire Solvent
Slide glass Ag 2 μm
Ti 0.035 μm
Fig. 2. Schematic illustration of die bonding using Ag direct-bonding.
As a comparison material, Ag paste which consists of two
kinds of micrometer-sized Ag particles was used. AgC239
(Fukuda Metal Foil and Powder Company Ltd., Kyoto, Japan)
flakes had a median particle diameter of 8 µm and FHD
(Mitsui Mining and Smelting Company Ltd., Tokyo, Japan)
had a round particle shape with a median particle diameter of
0.3 µm. The microstructures of the Ag particles are shown in
Fig. 1. To obtain a stable viscous paste, the mixed Ag particles
were dispersed in a high boiling point solvent prepared from
a mixture ratio of 2-ethyl 1, 3 hexanediol (boiling point:
244 °C)/diethylene glycol monobutyl ether (boiling point:
230.6 °C) = 80/20 w/w. Ag particles were used with a
composite ratio of AgC239/FHD = 80/20 w/w, and the content
of Ag particles in the paste was fixed at 92.6 wt%.
B. Direct Die-Bonding of the LED Die
A volume of 2-ethyl 1, 3 hexanediol solvent large enough to
coat the bottom face area of the LED die was added dropwise
on the die mounting substrate (i.e., the Ag-coated slide glass)
using the pin transfer method. The LED die, which also has
an Ag coating on the bottom face of the sapphire substrate,
was then placed face up in the organic solvent using vacuum
tweezers. A schematic illustration before sintering is shown in
Fig. 2.
In the pressureless direct bonding of mating Ag layers, it
is expected that the roughness of the bonded faces could have
substantial influence on the capability of bonding. The Ag
sputtered layer was coated on the surface of the slide glass
with smoothness of, Ra = 0.09 µm. The LED die could be
temporarily fixed to the die mounting substrate by the surface
tension of the organic solvent. Heat-treatment was carried
out from room temperature up to 200–240 °C. On heating,
the solvent was carefully evaporated at 120 °C. Finally, the
assembly was heat-treated at 200–240 °C for 2 h.
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549
7
Ag–Ag direct bonding
6 Micrometer-sized Ag particles
past (AgC 239/FHD)
Bonding strength/Kgf
5
3
2
1
0
190 200 210 220 230 240 250
Temperature/ °C
Fig. 3. Relationship between the sintering temperature and bonding strength
of the Ag sputtered layer for direct bonding of LEDs.
C. Analyses
The bonding strengths were measured as die-shear strengths
using a Dage 4000 Multi-purpose Bondtester (Dage Precision
Industries Ltd., Aylesbury, U.K.), following the MIL-STD 883
standard.
X-ray diffraction (XRD) patterns were recorded on a
Rigaku RINT-2500V diffractometer (Rigaku Corporation,
Tokyo, Japan) at 40 kV and 300 mA.
III. R ESULTS AND D ISCUSSION
A. Temperature Dependence of Bonding Strength of Ag–Ag
Direct Bonding
For micrometer-sized Ag particles sintered at low-
temperature with oxygen gas absorption, it was considered
that the mating surfaces of the resulting micrometer-sized
thickness Ag layers are expected to bond to each other at the
same low-temperature in the presence of oxygen. The bonding
strength of the Ag bonding layer formed by direct bonding of
the Ag sputtered layer as a function of bonding temperature,
is shown in Fig. 3, and compared with that of the paste of
AgC239/FHD.
The Ag direct bonding showed bonding strengths have a
large scatter in the temperature range of 200–220 °C. Some
of the Ag layers formed by direct bonding could not achieve
stable bonding. These can be attributed to contact failure; pos-
sibly too much localized contact prevents uniform bonding at
the interface. When the sintering temperature rises to 240 °C,
such contact failure could be eliminated and good bonding was
achieved. The bonding strengths exceeded the measurement
maximum scale (5 kgf) of the measuring apparatus used. When
this strength level was reached, the fracture mode after die-
share testing was not a fracture of the Ag bonding layer but
that of interfaces of the Ag bonding layer and the substrates. It
is supposed that the Ag bonding layer has strength near bulk
Ag (approximately 170 MPa).
From the results, it can be concluded that the low-
temperature sintering of micrometer-sized Ag particles as
previously reported [8], is not a phenomenon limited only
to micrometer-sized Ag particles, and this low-temperature
550 IEEE TRANSACTIONS ON COMPONENTS, PACKAGING AND MANUFACTURING TECHNOLOGY, VOL. 2, NO. 4, APRIL 2012

6
Sapphire (LED die)
5
2 μm Large Ag grain

Bonding strength/Kgf
4

2 μm Void 3

1
Slide glass
0
0 0.2 0.4 0.6 0.8
Roughness Ra/μm
5.0 kV 8.0 mm × 10.0 k YAGBSE 5.00 μm
Fig. 6. Relationship between the surface roughness of the Ag sputtered layer
Fig. 4. SEM image of the cross section of an Ag–Ag direct bonding interface and bonding strength (250 °C–2 h).
bonded at 240 °C.

7
Ag grains were also found along the bonding line. These
large grains indicate abnormal grain growth during the low-
6 temperature bonding process.
Bonding strength/Kgf

5
4
3 process is the same as that in the low-temperature sintering
2 of oxygen concentration in the sintering atmosphere and the
1 bonding strength was evaluated. The bonding strength as a
0 in Fig. 5. The bonding temperature was found to be 250 °C,
0 5 10 15 20
Oxygen concentration/%
Fig. 5. Influence of oxygen concentration in the atmosphere on the bonding
strength (250 °C–2 h).
sintering could be universally applicable to all kinds of Ag
materials, coating or bulk. Generally, as the solid-state dif-
fusion bonding of metals is hindered by oxide formation
on the metal surfaces, the investigation of solid-state bond-
ing of such metals in an oxygen rich atmosphere has not
been carried out actively. There have only been a limited
numbers of reports on the solid-state bonding of Ag–Ag in
inert gas [9], [10]. Most of the results, however, showed
that higher temperatures are required to achieve a substan-
tial bonding strength. For instance, the solid-state diffusion
bonding between Ag sputtered layers is typically achieved
at 400 °C and pressure of 207 MPa. Thus, the current low-
temperature bonding of Ag sputtered layers, i.e., at 240 °C,
in a pressureless atmosphere is a quite unique and interesting
phenomenon.
B. Observation of a Bonding Interface
A cross-sectional SEM image of the Ag–Ag direct bond-
ing interface, which was bonded at 240 °C, is shown in
Fig. 4. Even though several small voids were observed along
the bonding line, it is noteworthy that bonding remarkably
progressed at low-temperature without any pressure. Large
C. Oxygen Concentration Influence of Ag–Ag Direct Bonding
To confirm whether the role of oxygen in the direct bonding
of micrometer-sized Ag particles [7], [8], the relationship
function of oxygen concentration in the atmosphere is shown
25
which is considered from the result in Fig. 4 to be a sufficiently
high temperature.
The influence of oxygen concentration on the bonding
strength is clearly observed. The bonding strength increased
very sharply from 0% to 2% and, beyond 2%, the bond
strength became almost saturated. This tendency corresponds
well with the result for the low-temperature bonding of the
micrometer-sized Ag particles paste [8]. From this result, it is
summarized that the bulk-sputtered Ag coating can also form
intimate solid-state bonding at low-temperature in the presence
of oxygen above 200 °C.
D. Influence of Surface Roughness on Bonding Strength
The relationship between the surface roughness of a sub-
strate and the bonding strength was evaluated by roughening
the surface of the Ag sputtered layer. The Ag sputtered surface
on the slide glass was ground by using different grades of
silicon carbide sandpaper. After grinding, die-bonding was
carried out in air at 250 °C for 2 h. The result is shown
in Fig. 6. The bonding strength continuously decreased as
the surface roughness increased up to Ra = 0.5 µm. Thus,
it is clear that the bonding strength depends on the surface
roughness, which can be attributed to the contact area of the
bond face. In pressureless direct bonding, especially, the initial
contact area is greatly influenced by the surface roughness of
the bond faces. Thus, the surface roughness of the Ag sputtered
layer is one of the most important parameters in controlling
the quality of the die-bonding.

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KURAMOTO et al.: LOW-TEMPERATURE AND PRESSURELESS Ag–Ag DIRECT BONDING 551

25000 in Fig. 8. The average diameter of the initial Ag grains

Ag (111)
20000 was about 173 nm, which grew to an average diameter of

Intensity
15000 about 255 nm by heating in both atmospheres. The apparent
10000
difference observed in Fig. 8 is their surface morphologies.
5000 Ag (200) Ag (220)
0 The surface of the Ag grains after heat-treating in air was
15 25 35 45 55 65 75
2θ/deg. found to be much rougher than that heat treated in nitrogen.
In addition, as seen in Fig. 4, the abnormal grain growth at
(a)
the contact area is remarkable. Huge Ag grains larger than a
25000 few µm in size were observed along the bonding line. It is
Ag (111)
20000 supposed that Ag grains with larger area contacting air in the
Intensity
15000 Ag sputtered layer generate a crystal growth preferentially by
10000
oxygen adsorption, and the crystal growth would be able to
5000 Ag (200) Ag (220) break a surface contamination layer. Therefore, it is considered
0
15 25 35 45 55 65 75 that the bonding is achieved.
2θ/deg.
Dannenberg et al. reported that the grain growth of the Ag
(b) sputtered films of nano-grains occurs from about 100 °C in
vacuum [11]. They found that coarsening of the Ag grains of
25000
Ag (111) 100 nm in diameter begins at temperatures of approximately
20000
100 °C, and quickly reaches a plateau after a few 10 seconds.
Intensity

15000
10000
Even at 200 °C, grain growth stopped immediately at around
5000 Ag (220)
200 nm in grain size. Their observation is different from the
Ag (200)
0
15 55 75
present experiment primarily on two points. Grain growth of
25 35 45 65
2θ/deg. Ag is far more significant than their vacuum annealing and
(c)
the influence of oxygen in the grain growth near the surface
of the Ag grains is apparent, as shown in Fig. 8. Thus, the
Fig. 7. Morphology changes depending on heating atmosphere (SEM). abnormal grain growth with the interaction between Ag and
(a) Initial appearance and XRD result of the Ag sputtered surface. oxygen at the contact surface has a key role in the present
(b) After heating in nitrogen atmosphere (250 °C–2 h). (c) After heating in
air (250 °C–2 h). bonding process.

(a) (b)
Fig. 8. Cross-sectional TEM images of Fig. 7(b) and (c). (a) Heating in
nitrogen (250 °C–2 h). (b) Heating in air (250 °C–2 h).
E. Observation of Morphology Changes of the Ag Sputtered
Surface
To understand the mechanism of low-temperature bonding
or sintering of Ag materials, morphological observation of the
Ag sputtered surface at elevated temperatures was carried out.
SEM images of the Ag sputtered surface heated at 250 °C, both
in air and in nitrogen, and their XRD measurement results are
shown in Fig. 8.
From the comparison of Fig. 7(b) and (c), the change of
the surface of the Ag layer heated in air is as significant as
that in nitrogen. It can be deduced that the Ag grains of the
sputtered layer maybe near the surface exhibit abnormal grain
growth in the presence of oxygen. On the contrary, the XRD
patterns in Fig. 7(a)–(c) did not show any significant change,
which indicates that no oxidation of Ag occurred when Ag
was heated in air.
Cross-sectional transmission electron microscopy (TEM)
images of the specimens in Fig. 7(b) and (c) are shown
IV. C ONCLUSION
In this paper, a unique solid-state bonding method was
developed for die-attaching high-power LEDs and laser diodes.
The method can provide excellent thermal resistance and
electric resistivity because of the tight bonding at the interface
when they are bonded at temperatures above 240 °C in air. The
results are summarized as follows.
1) A novel solid-state low-temperature and pressureless
direct bonding method of substrates with an Ag sput-
tered layer having a thickness of micrometer size was
developed. The bonding strength is high, exceeding that
obtained with the micrometer-sized Ag particles paste.
2) The bonding strength was greatly influenced by the
oxygen concentration in the atmosphere. The bonding
strength increased with increasing oxygen concentration.
To obtain a high and stable bonding strength, an oxygen
concentration of greater than about 2% was required.
3) The bonding strength of the direct bonding depends on
the surface roughness of the Ag sputtered layer. The
bonding strength decreased with a roughening of the
Ag surface.
4) The Ag sputtered surface, with heating in air, exhibits
abnormal grain growth along the bonding line as
compared with that in nitrogen.
Thus, in Ag direct bonding in air, the Ag surface adsorbs
oxygen remarkably beyond 200 °C, which was then followed
by abnormal grain growth near the contact surface of Ag.
Although it is not clear what impact this has on the bonding

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552 IEEE TRANSACTIONS ON COMPONENTS, PACKAGING AND MANUFACTURING TECHNOLOGY, VOL. 2, NO. 4, APRIL 2012
mechanism of Ag–Ag with oxygen at microscopic scale, it is
quite likely that Ag-O interactions, i.e., a redox reaction, can
accelerate surface diffusion of Ag resulting in the abnormal
grain growth of Ag along the mating faces.
It is also noteworthy that die-attaching with the low-
temperature pressureless bonding method using Ag for LEDs
can be applied without changing the current die-bonding facil-
ities of LEDs. This procedure is useful as a die-attach method
that can substitute high-temperature, high-lead soldering.
ACKNOWLEDGMENT
The authors would like to thank their colleagues for their
contributions.
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Masafumi Kuramoto received the M.S. degree in
applied chemistry from the University of Tokushima,
Tokushima, Japan, in 1987.
He was with New Japan Chemical Company, Ltd.,
Kyoto, Japan, from 1987 to 1995. Since 1996, he
has been engaged in design on light emitting diodes
packaging materials with Nichia Corporation, Anan,
Japan.
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Teppei Kunimune received the B.S. degree from
the University of Tokyo, Tokyo, Japan, in 2005.
He joined Nichia Corporation, Anan, Japan, in
2005. He worked on device technology of light
emitting diodes (LEDs) from 2005 to 2009 and has
been working on packaging technology of LEDs
since 2010.
Satoru Ogawa received the B.S. degree in mechan-
ical engineering from the University of Yamaguchi,
Yamaguchi, Japan, in 1988.
He was with Toyota Auto Body Corporation,
Ltd., Aichi, Japan, from 1989 to 1991. He is cur-
rently a Subsection Chief with the Light Emitting
Diodes Production Division, Nichia Corporation,
Anan, Japan.
Miki Niwa received the Dr.Eng. degree from the
University of Tokushima, Tokushima, Japan, in
2008.
He was with Nichia Corporation, Anan, Japan,
from 2008 to June 2010. Since July 2010, he has
been an Assistant Professor with the University of
Tokushima.
Keun-Soo Kim was born in Korea in 1970. He
received the M.S. degree from Changwon National
University, Changwon, South Korea, in 1998, and
the Dr.Eng. degree from Osaka University, Osaka,
Japan, in 2003.
He became an Assistant Professor with the Insti-
tute of Scientific and Industrial Research, Osaka
University, in 2007, and an Assistant Professor with
the Fusion Technology Laboratories, Hoseo Univer-
sity, Asan, South Korea, in 2011. He has worked on
diffusion in metals for several years and recently he
is focusing on interconnection and printing technologies for green electronics
packaging.
Katsuaki Suganuma received the Dr.Eng. degree
from Tohoku University, Miyagi, Japan, in 1982.
He was a Research Assistant with the Institute
of Scientific and Industrial Research (ISIR), Osaka
University, Osaka, Japan, from 1982 to 1986, an
Associate Professor with National Defense Acad-
emy, Kanagawa, Japan, from 1986 to 1996, and a
Professor at ISIR in 1996. He has been the Deputy
Director of ISIR since 2010. He has focused on lead-
free soldering, conductive adhesives, and printed
electronics.