Special Issue

Challenges to New Technologies and New Products

Advanced Analysis Technology for New Material
and Product Development
Hirokazu Sasaki*1, Hideo Nishikubo*1, Shinsuke Nishida*1, Satoshi Yamazaki*1,
Ryusuke Nakasaki*2, Takemi Isomatsu*2, Ryuichiro Minato*3, Kohei Kinugawa*3,
Akihiro Imamura*3, Shinya Otomo*4, Yujin Hori*5, Kiyoshige Hirose*6, Satoshi Anada*7,
Kazuo Yamamoto*7, Tsukasa Hirayama*7, Jun Yamasaki*8, Naoya Shibata*9,
Yojiro Oba*10, Masato Ohnuma*11

Several cases using advanced analysis technology including electron microscope, synchrotron radiation, and surface analysis for various new materials/
products are introduced. Electron holography and the Differential Phase Contrast-Scanning
Transmission Electron Microscopy (DPC-STEM) were used for the analysis of a semiconductor
laser diode for optical communication. 3D analysis with Focused Ion Beam-Scanning Electron
Microscopy (FIB-SEM) was utilized for analyzing winding wire with a micro cellular coating. The
Small Angle X-ray Scattering (SAXS) method was used at Super Photon-ring-8-GeV (SPring-8)
for analyzing a coated superconductor tape and a copper alloy. The surface analysis method ofHard X-ray Photoelectron Spectroscopy (HAXPES) was utilized for analyzing the AuSn solder.

ABSTRACTINTRODUCTION
1.1. INTRODUCTION
Furukawa Electric (FEC) offers a wide variety of products
and fosters next-generation business based on the coretechnologies of photonics, polymers, metals, and highfrequency electronics. Examples in the photonics field
include optical fibers, products related to the semiconductor laser diode etc. In the field of polymer technology
application, various products include the tapes for semiconductors as well as various foamed products. In themetal field, typical products include copper alloys, oxygen-free copper, and aluminum blanking material for
memory disks.
At the actual sites where new products are developed,
it is important to have a thorough understanding of thematerials that define the products. The relevant characteristics can be obtained by properly understanding compound semiconductors (GaAs, InP, etc.) in the case of thesemiconductor laser diode, copper and aluminum in the
Advanced Technologies R&D Laboratories, R&D Division
Automotive Products & Electronics Laboratories, R&D
Division*3
Furukawa Fitel Optical Device Co.,Ltd*4
Corprate Planning Department, Strategy Division*5
HR Departmet, Strategy Division*6
Marketing Relationship Management Department, Marketing
Initiatives & Business Development Department, Global
Marketing Sales Division*1*2

case of metal products, and the adhesive compound in
the case of the tape used for semiconductors.
In order to understand each material, the Analysis
Technology Center at FEC has been analyzing the materials for the products manufactured in the plants and underdevelopment by using various analytical equipment. An
overview of the roles undertaken of the Analysis
Technology Center is provided in Figure 1. In the case of
products currently under development, the elucidation of
the mechanism behind the function expression and thecharacteristics of the new materials is carried out andthen utilized as design guidelines for the new products.
Also, when any type of problem occurs at the plant, weinvestigate the cause immediately from the viewpoint ofmaterial analysis and facilitate the problem solving.

Japan Fine Ceramics Center
Osaka University*9
The University of Tokyo*10
Japan Atomic Energy Agency*11
Hokkaido University*7*8

Furukawa Electric Review, No. 50 20192

Advanced Analysis Technology for New Material and Product Development

Provide products
based on science

Plant

Laboratory

New
product

Customers

Mechanism
analysis on
newmaterials

Immediatetroubleshooting
Utilizingstate-of-the-art
science.

State-of-the-art
electronmicroscope

Analysis Technology Center
500m

SPring-8(large synchrotron radiation facility)

External research facility
Figure 1 Roles of the analysis technology center.

In recent years, advanced analysis equipment has
become more expensive, and it is often impractical toown every single piece of equipment that is needed.
When our equipment is not sufficient for an analysis, wetypically borrow an advanced electron microscope from a
university or a synchrotron radiation facility such as Super
Photon-ring-8-GeV (SPring-8). An important objective of
the Analysis Technology Center is to provide customers
with products based on science through reliable material
analysis. To this end, we collaborate with universities andpublic research institutes that possess advanced analysis
equipment and technology.
Thus far, we have applied advanced material analysis
technology to the development of new materials andproducts by collaborating with many research institutes.
The semiconductor analyses by electron holography and
DPC-STEM discussed in this paper are collaborative projects with the Japan Fine Ceramics Center (JFCC) and the
University of Tokyo, respectively. We carried out precise

analysis of the p-n junction in collaboration with Osaka
University. Our analyses of copper alloy and coatedsuperconductor tape by SAXS utilizing SPring-8 are theresults of research with Hokkaido University, the Japan
Atomic Energy Agency, and Kyoto University.
Today, research facilities and analytical devices in universities and public institutions are well organized for private companies to use, and we utilize a lot of equipment
to analyze various materials. We have used mainly
SPring-8 and the Aichi Synchrotron Radiation Center for
analysis by synchrotron radiation. We have also worked
with the Japan Proton Accelerator Research Complex(J-PARC) for analysis using neutrons. For advanced electron microscopy and surface analysis, equipment owned
by JFCC, the University of Tokyo, and Nagoya University
is regularly utilized. In this paper, we introduce some
application examples using advanced analysis technologies to analyze a number of new materials and products.

Furukawa Electric Review, No. 50 20193

Advanced Analysis Technology for New Material and Product Development

PN

100 nm（b）-0.4

P-GaAs

N-GaAs-0.3

phase
potential

-0.2
-0.1

1.0

0
0.1

0.5

0.2
0.3
0.4
470

1.5
Potential (eV)An electron microscope is used to observe products byenlarging the view from several thousands to several million times by means of electron beams with a wavelength
shorter than light. It is possible to observe the surface ofa specimen with Scanning Electron Microscopy (SEM)
and the inside of a specimen at a high magnification withTransmission Electron Microscopy (TEM). Which one touse is selected according to the purpose.
In this paper, electron holography and the DPC-STEM
method are introduced as case studies of TEM, and as an
example of SEM, a case of 3D analysis with Focused Ion
Beam (FIB) is introduced.
2.1 Precise Analysis of Semiconductor p-n Junction
by Electron Holography
As one method of TEM, the use of electron holography toobserve the potential in a semiconductor initially proceeded as research with Si semiconductors.1)-3) In order
to apply this technique to compound semiconductors, ajoint research between JFCC and FEC was set up andsuccessful observations with GaAs and InP were performed in 2006.4) More recently, it is being applied to theobservation of devices such as semiconductor laser
diodes.5) At the beginning of this research, the observation was mostly with the magnification of several thousands to tens of thousands of times. The resolution in theconventional electron holography was insufficient toobserve the electric potential distribution of the semiconductor at a higher magnification, so we applied thephase-shifting method based on a double-biprism electron holography. In doing so, we have achieved high-resolution potential distribution observation on the p-n junction of GaAs.
A phase image with the electron holography is shown in
Figure 2. The specimen was GaAs and the dopant concentration of the p-type semiconductor and the n-typesemiconductor was 1×1019 cm–3 for each. From this dopant concentration, approximately 20 nm of the depletion
layer width was expected. Using TEM (Hitachi HF-3300
EH; owned by JFCC), observation was conducted under
the double-biprism condition, and the phase was reconstructed with the phase-shifting method. As shown in thephase image in Figure 2(a), the contrast difference clearly
appears in the p-n junction. Regarding the area enclosedby the frame, the phase profile was created as shown in
Figure 2(b). The potential distribution estimated from thedopant concentration is shown on the same graph. Since
these two profiles are in close agreement, we can see
that, by using electron holography, the potential change
in the p-n junction with a 20-nm-wide depletion layer canbe observed in the high spatial resolution.

（a）Phase (rad)NEW PRODUCTANALYSIS
USING
2.2. OUTLINES
OF THEAUTOMOTIVEELECTRON MICROSCOPY
RADAR

0
480

490

500
510
Distance (nm)

520

530

Figure 2 Precise analysis of the GaAs p-n junction with phaseshifting electron holography.
(a) Phase image and (b) phase profile across the p-njunction.

On the basis of this result, we attempted to observe
how the electric potential and the electric field change byapplying a voltage to the p-n junction. In this experiment,
electrodes with low contact resistance were formed on
the surface of the semiconductor. We utilized the manufacturing process of the semiconductor laser diode in
FEC for the electrode manufacturing.
The analysis results of the electric field profile areshown in Figure 3 (a). The applied voltage was varied from
–0.3 to 0.5 V, and we successfully detected the associated changes in the electric field profile at the p-n junction.
In addition, we were able to observe the depletion layer
width caused by the voltage change. These results are inclose alignment with the theoretical expectation, indicating that the experiment was properly performed.6) Thus,
by using electron holography, the electric potential andthe electric field can be directly visualized in high special
resolution of several nm, and as such, it can be used forthe development of new semiconductor devices.

Furukawa Electric Review, No. 50 20194

Advanced Analysis Technology for New Material and Product Development（a） 1.4E+08

2.2

W

1.2E+08

Elecｔricｆield [MV/cm]

-0.3V
-0.2V
-0.1V

1.0E+080V
0.1V

8.0E+07

0.2V
0.3V

6.0E+07

0.4V
0.5V

4.0E+072.0E+07

0.0E+00-50 -40 -30 -20 -10 0 10 20 30 40 50
Distance (nm)30（b）

Depletion layer width W [nm]2520

W (Va) = -4Va + 24

15
10
5
0
-0.5

0.0

0.5

Applied voltage Va [V]Figure 3 Precise measurement of electric field across
GaAs p-n junction by in situ biasing and electron
holography.
(a) Change in electric field profiles and (b) depletion
layer width across p-n junctions.

（a）PAnalysis of Semiconductor Laser Diode byDifferential Phase Contrast (DPC) Method
Thanks to advancements with STEM, the electron beam
can now be focused to the utmost limit, and atomic visualization is becoming a routine analysis. The DPC method, which is a method of STEM, has also shown significant progress in atomic resolution observation.7) The
University of Tokyo and FEC collaborated to observe the
GaAs p-n junction in order to evaluate the electric field insemiconductors with DPC-STEM. With the cooperation of
JEOL Ltd., we found the optimal observation condition
for the p-n junction and succeeded in observing it.8)
Today, DPC-STEM is becoming a common method.
Figure 4 (a) shows the DPC-STEM image of a GaAs p-njunction. The JEOL 2100F TEM equipped with an aberration corrector (owned by the University of Tokyo) wasused. The camera length was 140 m and the beam diameter was 12 nm. We found that the p-n junction could beclearly observed at the center of the DPC-STEM image.
The arrows in the figure indicate the interfaces where thedopant concentrations changed, and as shown, evensmall potential changes could be observed.
With this method, devices having a 2D shape can beobserved. A part of the semiconductor laser diode for the
optical communication is shown in Figure 4. In the figure,(b) shows the image captured by the Annual Dark Field(ADF)-STEM method, which is a conventional method. In
this image, the interface between the p-type semiconductor and the n-type semiconductor cannot be observed. In
contrast, in the observation result by DPC-STEM, shownin (c), the 2D p-n junction that could not be observed in
the ADF-STEM image is clearly visible. In this example,
the device under observation was a characteristicallydefective item; specifically, the p-n junction shape was
not as designed.5) Thus, through the p-n junction observation using DPC-STEM, defects in products can be
identified.

（b）

（c）

p

p

n

n

N

n

n
100 nmp

100 nmp

200 nmFigure 4 Observation by DPC-STEM on p-n junction and semiconductor laser diode.
(a) DPC-STEM image of the p-n junction region in GaAs. (b) ADF-STEM
and (c) DPC-STEM image of the semiconductor laser diode.

Furukawa Electric Review, No. 50 20195

Advanced Analysis Technology for New Material and Product Development

In addition to the DPC-STEM and electron holography
introduced thus far, semiconductor observation technology with the electron microscope has also been progressing. Research on electron diffractive imaging 9), 10) ,4D-STEM11), the shadow method12), etc. as new potentialand electric field observation methods is currently underway. If we take advantage of these methods in a complementary way, further detailed progress in device analysis
will become possible.
2.3 3D Analysis of Winding Wire with Micro Cellular
Coating by FIB-SEM
Typical 3D analysis methods on the micron order or lessinclude X-ray tomography, 3D analysis using FIB-SEM,
TEM tomography, and the 3D atom probe method. The
observable size of a specimen and its spatial resolution
are different from each other, so it is necessary to select asuitable method for the purpose of the observed material.
In this section, we introduce 3D structural analysis using
FIB-SEM for the enamel part of the enameled winding
wire containing micro-sized bubbles.
The winding wire with micro cellular coating can
improve the partial discharge inception voltage by controlling the volume ratio and the size of the bubbles, andit contributes to the size reduction and the increase of the
motor output.13) To ascertain the shape distribution of the
bubbles, 3D images were taken using FIB and SEM. FIB
can process the cross section at a high accuracy on the
nm order with the focused ion beam, and furthermore, by
irradiating the ion beams repeatedly to the processedcross section, a new cross section can be prepared.
Utilizing this feature, as shown in Figure 5(a), by periodically repeating the cross section preparation with FIB andSEM observation, the 3D information of the material canbe obtained.
When bubbles come into contact with each other, they
are sometimes separated by walls thinner than 0.1 μm.
Therefore, in the observation of bubbles containing
enamel, the performance of the electron microscopemounted on the FIB-SEM is important. We therefore used
an orthogonal type FIB-SEM (MI4000L; owned by Nagoya
University), and instrument in which the FIB and SEM columns are orthogonally arranged. Since orthogonal FIBSEM can keep the field of view almost completely steady,even when 500 or more section images are taken, it ispossible to obtain 3D images with a wider range in thedepth direction. The mounted SEM has a spatial resolution of 10 nm or less even under the observation condition of the low acceleration voltage of 3 keV or less,which is a sufficient performance for observing bubbles
containing enamel.
An example of the SEM image is shown in Figure 5(b).
The bubble size is several μm and bubbles with various
shapes and sizes can be observed. However, observationfrom a single cross-section cannot provide information on
the depth direction, which means that accurate structural
information cannot be obtained. Therefore, in order toperform 3D observation, the section processing was per-formed using the FIB at 100-nm pitch, and 500 sheets of
SEM images were obtained. The luminance information,
which was obtained from the serial cross-sectional SEM
images in the range of 50μm with respect to the depth
direction, was converted into 3D pixels called voxels. This
resulted in the 3D image shown in Figure 5 (c), completewith a visible 3D bubble shape formation.
By utilizing this 3D analysis method, the partial discharge inception voltage can be improved and the innovation of motor technology will thus be possible.

SEM observation（a）Conductor
Enamel coating

FIB processing

（b）

（c）

Figure 5 FIB-SEM 3D analysis of winding wires with micro
cellular coating.
(a) Schematic diagram of FIB-SEM analysis (b) Cross
section SEM image and (c) 3D reconstruction of the
micro cellular coating.

Furukawa Electric Review, No. 50 20196

Advanced Analysis Technology for New Material and Product Development

PRODUCTANALYSISANALYSIS USING SYN3.3. PRODUCTSYNCHROTRONRADIATION
CHROTRONRADIATION
Synchrotron radiation is a powerful electromagnetic wave
emitted by charged particles accelerated to nearly the
speed of light, with features including high brilliance,
polarization, parallelism, pulsed light emission, and energy selectivity. Utilizing these characteristics of light, timeresolved measurement and X-ray absorption fine structure spectroscopy using X-rays near the absorption edgeof a specific element are utilized in material analysis.
In this paper, we introduce cases of anomalous smallangle X-ray scattering (ASAXS), time-resolved SAXS
measurement, and HAXPES utilizing these features.
3.1 Analysis of Artificial Pin in Superconducting
Material by ASAXS Method
Since superconducting material has zero electric resistance at ultralow temperatures, it can contribute to a
power saving environment due to its low electric power
loss. It is also expected to be applied in products such as
high voltage cables. In order to develop a tape with ahigh critical current density (Jc), control of the flux quantum is necessary. When the superconductor tape turns
into a coil shape and is used as a strong magnetic field
generator, a strong magnetic field is applied to the tape.
When it is applied to the superconductor material, flux
quantum is formed. With the current flow, the flux quantum moves with the Lorentz force, generating heat, andhence resistance is created. Therefore, it is necessary to
pin the flux quantum into an appropriate normal conducting layer. Since around 2004, the development of an artificial pin to artificially introduce the pinning site into thesuperconducting material has been pursued.14), 15) One
promising example is a rod-like normal conducting partwith a diameter of several nm in the vertical direction of
the thin layer that is formed as an artificial pin.16) If thisartificial pin can be introduced as designed, the superconducting state can be maintained even in a high magnetic field, and a strong magnetic field then be generated.
In light of this background, material analysis on whether
or not the artificial pins can be created as designed isnecessary. For the artificial pin, although the analysis
method for observation using TEM (as shown in Figure 6(a)) is common, the observation area is as narrow as several μm, which is insufficient for the quantitative evaluation of size and distribution through the entire tape.
Therefore, in order to establish a highly accurate quantitative evaluation method, we performed a nano-rod artificial
pin evaluation using the small-angle scattering method.
In small-angle scattering, X-rays or neutrons are irradiated to materials and those that scatter at a small angleof 10 degrees or less are analyzed to obtain average
information of the microstructures. Specifically, information on the average size and orientation of the nanoparticles and the secondary phase contained in the materials
is obtained. It is effective for the material analysis to be
used in conjunction with the TEM.

For artificial pins including heavy atoms such as Au,
SAXS is applied as the artificial pin for the superconductor tape.17) However, the X-ray contrast of the practical
BaZrO3 in (Gd, Y) BaCuO is low due to the small difference of electron density from (Gd, Y) BaCuO of thesuperconductor phase, and sufficient scattering intensity
cannot be obtained. Therefore, we aimed to establish aquantitative evaluation method of the size and dispersion
state of the artificial pins using ASAXS targeting Zr.
ASAXS targets anomalous X-ray scattering phenomena
occurring in the energy region near the absorption edgeof a specific element, and it is possible to change thescattering contrast in the small angle scattering measurement.
For the ASAXS measurement, we used a SAXS device
installed in BL19B2 at SPring-8. Figure 6 (b) shows theanomalous small-angle X-ray scattering results of (Gd,Y)1Ba2Cu3O7 thin film in which 25% of Zr has been added.
Profiles 1–4 in Figure 6 (b) show the measurement results
at 17.885, 17.985, 17.990, and 17.995 keV, respectively.
The Zr-K absorption edge is 17.998 keV. A shoulder wasobserved in the vicinity of q = 0.2–1.0 nm–1 (indicated by
the arrow in (b)), and we confirmed the formation of anano structure of several nm in the superconductor
phase. Compared with profile 1, which was sufficiently far
away from the absorption edge, peak intensities around q= 0.3 nm–1 increased for profiles 2, 3, and 4. These results
suggest that the scattering of these peaks was caused by
the artificial pins due to BaZrO3 containing Zr.
The measurement results of the specimens with Zr
addition amounts of 7.5%, 15%, 20%, and 25% areshown in Figure 6 (c). Using these results, the rod diameter was estimated with the unified fit.18), 19) As shown in
Figure 6 (d), although the diameter tended to increase as
the Zr concentration increased, there was no significant
difference between the 20% and 25% specimens. Thus,
by utilizing ASAXS, it is possible to analyze the artificial
pins in the superconductor phase with a high accuracy,
thus contributing to the development of superconductor
wire with high critical current density.

Furukawa Electric Review, No. 50 20197

Advanced Analysis Technology for New Material and Product Development（a）（b）1001 17.885 keV
2 17.985 keV
3 17.990 keV
4 17.995 keVIntensity (arb. unit)

10-1

10-2

10-3

10-4
50 nm
10-5
10-1

Intensity (arb. unit)

10-1

10-2

10-3

10-4

10-5
10

3

4 5 6 7 89
100
q (nm-1)

1020
Zr content（%）2（d） 5.0
7.5 %
15 %
20 %
25 %

-1

2

3

4 5 6 7 89
100
q (nm-1)

2

4.8
Radius of gyration (nm)（c）100

2

4.6

4.4

4.2

4.0

0

30

Figure 6 Characterization of artificial pin in the superconductor tape by ASAXS.
(a) TEM image of artificial pinning center (b) Energy dependence of the scattering profiles of Zr-added
samples. (c) Anomalous small-angle X-ray scattering profiles and（d）average diameter of artificial pinning
center in 25, 20, 15, and 7.5 mol% Zr-added samples.

3.2

In-situ Measurement of Cu-Ni-Si Precipitates by
Small-Angle X-ray Scattering
Recently, along with the miniaturization and weight reduction of electric devices such as portable devices and personal computers, the electronic parts used for them arealso becoming more miniaturized and their performancesneed to be improved. The performance required for thecopper alloys used in, for example, the conducting partsof connectors is also increasing. In order to prevent insufficient terminal strength and insufficient conductivity due
to the miniaturization of the terminals, materials withhigher strength and higher conductivity than their conventional counterparts are required. Cu-Ni-Si alloys cansatisfy these requirements, and as the TEM image in
Figure 7 (a) shows, the strength can be improved by finely
dispersing the Ni-Si based compound as a precipitate
into the Cu parent phase by heat treatment. In order toclarify what strengthens the precipitation, quantitativeevaluations of the precipitates on the size distribution andon the dispersion state are necessary. However, TEM

observation is restricted to local information and is thus
insufficient. Therefore, in order to obtain size informationof the precipitates of Corson alloy and information on
their growth process, in-situ SAXS measurement, which
can obtain average information, was carried out.
For this SAXS measurement, the SAXS device installed
at BL19B2 was used. We selected the x-ray energy of 18
keV, and a 2D position sensitive detector (PILATUS-2M)
was used as a detector. For the aging treatment, theHS1300g heating stage by Instec Ltd. was used. The
heating rate was set to 10°C/min. and the maximum
attained temperature was 500°C.
Figure 7 (b) shows the profile during heating. During thetemperature rise process, the shoulder changed to thelow-q side, and the precipitates coarsened. (c) shows the
profile change during isothermal holding time at aging
temperature 500°C. As time goes by, the scattering intensity increased and the shoulder shifted to the low-q side.
After four hours had elapsed, the profile did not appear
saturated, and it tended to increase further and to shift to
Furukawa Electric Review, No. 50 20198

Advanced Analysis Technology for New Material and Product Development

the low-q side. By proceeding with such data analysis indetail, the mechanism behind the nucleation and grain
growth can be clarified, which will be of great benefit in
the development of new copper alloys.
（a）Precipitates

5 nm

（b）

104

RT
100℃
200℃
300℃
400℃
420℃
440℃
460℃
480℃
500℃

Intensity (arb. unit)

103

102

101

100

10-1
10-1

（c）

2

3

4 5 6 78 9100
q (nm-1)

104

0 min
10 min20 min30 min40 min75 min
125 min
150 min
200 min
250 min

103
Intensity (arb. unit)

2

102

101

100

10-1
10-1

2

3

4 5 6 78 9100
q (nm-1)

3.3 AuSn Solder Oxide Film Analysis by HAXPES
X-ray Photoelectron Spectroscopy (XPS) is a surface
analysis method used to obtain information on the element species, the composition, and the chemical state on
the surface through the detection of photoelectrons emitted by irradiating a solid surface with X-rays. Since thesurface state of the components used in products contributes greatly to the bonding characteristics between
the components, it is very important to analyze the organic contamination layer, the thickness, and the chemical
state of the oxide layer on the surface of the specimen.
Changes in oxide layer thickness can be evaluatedfrom depth profiling analysis using Ar ion spattering.
However, the chemical state and the electronic state of
the sputtered surface are damaged by the sputtered ions,and there is a possibility that the original chemical state
and the original electronic state of the material to be analyzed may be altered. In addition, since depth profiling
analysis using ion spattering is a destructive analysis, inthe case of only one specimen (such as a defective or
faulty product), it is very difficult to perform the same oranother analysis again.
We therefore use Hard X-ray Photoelectron Spectroscopy(HAXPES), which offers greater sampling depth of analysis compared to conventional XPS, so as to perform theoxide layer thickness evaluation and depth profiling analysis nondestructively. Over the past ten years, HAXPES
experimentation utilizing the synchrotron radiation at
SPring-8 is readily available for corporate R&D and products development 20)-22), and FEC has also been conducting HAXPES measurement on BL46XU.
In this section, we report the analysis results for the
AuSn solder used for jointing members in various products. The specimen used for the analysis were two typesof AuSn solder (specimens A and B) with different Sn
oxide layer thickness. The oxide layer thicknesses
obtained from the depth profiling analysis by XPS wereca. 2 nm for specimen A and ca. 11 nm for specimen B.
Figure 8(a) shows the Sn3d spectrum obtained by measuring the surfaces of specimens A and B with XPS. The
XPS instrument we used was a Refurbished
ESCA5400MC (by Physical Electronics Inc.) owned by
FEC. The incident X-ray was the monochromatic Al Kα(1486.6 eV) and the take-off-angle was 75°. In specimen
A, two components of Sn oxide film layer and AuSn weredetected, but only the Sn oxide layer component was
detected in specimen B, and the underlying AuSn component was not detected.

2

Figure 7 Measurement of Cu - Ni - Si alloy precipitates size by
in-situ SAXS.
(a) TEM image (b) profile change during heating (c)profile change during isothermal holding time at 500
degrees.

Furukawa Electric Review, No. 50 20199

Advanced Analysis Technology for New Material and Product Development（a） x 104
12

CONCLUSION
4.4. CONCLUSION

Sn3d

Sn oxide

10
AuSn

c/s

8
6
4

Specimen A
Specimen B

2
0
505

500

495
490
Binding Energy (eV)

485

480

As discussed in this paper, by utilizing various advanced
analysis equipment and analysis technology in the field of
new material/new products development, we can obtain
information that is vital in determining the design guidelines. In addition, even in existing products, the advanced
analysis technology may play an important role in somecases. We will continue to develop new analytical technologies in order to provide highly reliable products thatare embraced by society.

（b） x 104
6 Sn3dSn oxide

5
c/s

4
3
2

AuSn
Specimen A
Specimen B

1
0
505

500

495
490
Binding Energy (eV)

485

480

Figure 8 Oxide film analysis of the AuSn solder surface by(a) XPS and (b) HAXPES.

The Sn3d spectrum obtained by measuring AuSn solder specimens A and B with HAXPES is shown in Figure8(b). The HAXPES measurement was performed using
BL46XU at SPring-8. The incident X-ray energy was
7939.0 eV and the take-off-angle was 80°. In the HAXPES
measurement, two components of the Sn oxide layer and
AuSn were detected not only in specimen A but also in
specimen B, in which only the Sn oxide layer was detected by XPS measurement. This means that nondestructive
thickness evaluation, chemical state analysis, and depthof analysis profiling analysis of the Sn oxide layer on
AuSn solder is possible with HAXPES due to its greater
sampling depth. By applying this technique, we are able
to clarify the component bonding mechanism used in various products.

ACKNOWLEDGEMENTS
A part of this work was supported by the project for promoting public utilization of advanced research infrastructure and the Advanced Characterization Nanotechnology
Platform of the University of Tokyo, and as well by
Nagoya University through the Nanotechnology Platformof the Ministry of Education, Culture, Sports, Science andTechnology (MEXT), Japan. A part of this work was supported by JSPS KAKENHI Grant Numbers JP26286049
and JP26600042. The synchrotron radiation experiments
were performed at SPring-8 with the approval of theJapan Synchrotron Radiation Research Institute (JASRI)(Proposal Nos. 2016B1790, 2014A1814, 2014B1942,
2015B1789, 2017B1803, and 2018B1655). A variety ofstate-of the-art research facilities and support systems
have been developed to clarify technical issues in theindustry, and we wish to thank and express our sincere
gratitude to the people concerned for the great benefits
this has provided our research.

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