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3D Investigation of the microstructure

modification in Hypereutectic Aluminum
Silicon (Al-30Si) Alloy

Article · April 2017

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 3D MICROSTRUCTURE OF HYPEREUTETIC ALLOY
3D investigation of the
microstructural modification
in hypereutectic aluminum
silicon (Al-30Si) alloy
A. Gourav Rao1, V. P. Deshmukh1, Leah L. Lavery2, Hrishikesh Bale2
1 Naval Materials Research Laboratory, India; 2 Carl Zeiss X-ray Microscopy, USA
INTRODUCTION
Contemporary high performance
structural materials are characterized
by their mechanical properties,
particularly the strength, ductility,
toughness, corrosion resistance, and
machinability required for fabricating
devices. However, improving one
property often occurs at the expense of
other desirable properties.
Hypereutectic Al-Si alloy is an
attractive class of engineering material
that finds application in many critical
electronic and defence purposes
because of its low coefficient of thermal
expansion (CTE), high electrical
conductivity, and light weight as
compared to other established alloys.
The common problems in these
alloys are inherent brittleness, low
formability, and catastrophic failure
due to the presence of a coarse primary
silicon phase which increases with
the increase in silicon content. In
the present work, a novel approach of
friction stir processing (FSP), a variant
of severe plastic deformation process, is
used for microstructural refinement1, 2.
The undesirable coarse primary silicon
particles (~200 µm) in an Al-30Si
cast alloy were refined to very small
primary silicon particles (~3 µm) via
FSP. Also through FSP the particle
orientation can be altered such that the
preferred directions of the particulates
are randomized.
The degree to which the
modification is achieved can be
controlled through the number of stir
processing passes3,4. The efficacy of FSP
is classically determined by observing
the microstructure using optical or
S4
scanning electron microscopy (SEM)
stereological techniques where the
particulates can be analyzed for shape,
size and distribution. However, images
acquired using both these 2D imaging
techniques do not fully represent
the material since the sub-surface
information of the material is not
revealed. 3D X-ray microscopy enables
the non-destructive investigation
of a material in three dimensions;
revealing the internal microstructure
and discerning features such as voids,
cracks and differences in density of the
bulk material.
Owing to its non-destructive nature,
samples used in 3D X-ray microscopic
investigations can further be subjected
Tomography and image analysis March/April 2017 | MicroscopyandAnalysis
Figure 1 Schematic
of FSP operation shows
a workpiece being
subject to FSP wherein
the tool is pushed
into the workpiece as
it rotates generating
enormous localized
heating from friction.
The rotational forces
and local heating lead
to microstructure
modification from
friction and intense
plastic deformation. (a)
text which refers to the
image / scan (b) further
text that relates to
second image etc
to more than one imaging modality
such as SEM, Electron Back Scattered
Diffraction (EBSD), Energy Dispersive
X-ray Spectroscopy (EDS) etc. to obtain
additional information, for example,
the elemental composition or the
crystal structure. In this present study,
results obtained on a FSP specimen
using X-ray microscopy are presented
to demonstrate the capabilities of the
technique.
FRICTION-STIR PROCESSING
Friction-stir processing (FSP) is a solid-
state process (localized melting) that
uses a third body tool to join or process
materials through intense, localized
plastic deformation. The confined
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 3D MICROSTRUCTURE OF HYPEREUTETIC ALLOY

Figure 2 (a) Picture included in the region being imaged.

of the sample before
milling to final
No further specimen preparation was
dimensions of 1 mm x required. The sample was mounted
1mm. The red square in a standard pin vice and imaged
highlights the region non-destructively in 3D using an X-ray
from which sample was microscope (ZEISS Xradia 520 Versa).
extracted. (b) Sample As seen in Fig 2a, the processed region
mounted in a pin-vice
for X-ray imaging. of the sample showed significant
reduction in the silicon particles in
comparison to the bulk cast alloy.
Characteristically the X-ray
attenuation contrast between
aluminum and silicon is extremely low
due to the small difference in atomic
weight. Furthermore, as the particle
dimensions are reduced in size the
contrast reduces significantly.
Using the microscope’s resolution-
at-a-distance (RaaDTM) feature
facilitated by the detector optical
components (Fig. 3a), the propagation
phase contrast (PPC) mode was engaged
by positioning the source and detector
far from the sample. PPC works on
the principle of refraction of X-rays at
the interfaces of different phases (for
example, crack-material or material-
Figure 3 (a) plastic deformation is generated by technology for the automotive and inclusion interfaces) within a given
Schematic of the X-ray utilizing a non-consumable rotary aerospace industries where new material. As the X-rays pass through
imaging setup in the
ZEISS Xradia Versa
tool that is forced downward into the materials need to be developed to the sample, the interaction with the
microscope shows the workpiece, which forms a localized improve resistance to wear, creep, and different phases of the material causes
arrangement of the heat zone due to friction as shown in fatigue. a distortion in the x-ray wavefront
source, sample and Fig.1. The continuous rotation of the proportional to the phase-shift
detector system. The tool in contact with the ‘soft’ heated NON-DESTRUCTIVE imposed by the refractive indices
detector assembly
consists of multiple
zone causes localized stirring of the 3D X-RAY IMAGING of the material constituents. The
magnification material, creating a microstructure A 5 mm pillar with a 1 mm x 1 mm propagating distorted X-ray wavefront
objectives that can be with finer grains, or in case of the cross section was prepared by milling generates Fresnel diffraction fringes
switched to achieve Al-30Si leading to finer grains as well out a bulk section of FSP Al-30Si in the images collected on the detector
the desired resolution. as size reduction and homogeneous sample (as shown in Fig. 2) using a (shown in the schematic of Fig.3b). The
(b) Comparison images dispersion of Si particles in the matrix. conventional mechanical mill. The amplitude of these fringes is magnified
show the different
contrasts achievable FSP is primarily used on aluminum, pillar was extracted from the interface at a distance farther away.
using absorption and most often on extruded aluminum region of the stir zone such that The Al-30Si sample was imaged in
phase contrast. The (non-heat treatable alloys) and regions of both the unaltered cast both absorption and phase contrast
schematic shows titanium alloys, and is a promising alloy and the refined Si from FSP were mode at a 3D spatial resolution of 1.35
an X-ray wavefront µm/voxel. Reconstructed data using
interacting at a material
interface leading to
absorption contrast alone was able to
the emergence of the clearly resolve silicon particles > 10
Fresnel fringes. The µm in the bulk alloy; however, very
amplitude of these few small particles (< 10 µm) exhibited
fringes intensifies as the sufficient absorption contrast to be
detector is moved away
from the sample
discerned in the FSP side of the sample.
Imaging the same region of the
same sample using the PPC mode
showed that the 2-3 µm particles were
easily resolved along with a higher
edge contrast around voids and larger
Si particles. A comparison of the
reconstructed slices obtained using
the two contrast mechanisms is shown
in Fig. 4. The 3D image stack from
a the phase contrast tomography was
used to determine the quantitative
b information of the silicon particles
dispersed in aluminum.
By using routine image processing
steps, including greyscale thresholding
and morphological operations, the data
was segmented into the base aluminum
material, silicon particles, and voids
using the visualization and image
processing package Dragonfly Pro v2.0
(Object Research Systems Inc, Montreal

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 3D MICROSTRUCTURE OF HYPEREUTETIC ALLOY
Figure 4 Cross-sectional slices from the reconstructed data Canada)5. After the segmentation step,
acquired from the Al-30Si sample show significant difference in the binarized images were loaded
contrast between the absorption and phase contrast datasets. The into the particle analyzer module
unique advantage of using phase contrast is exemplified by minute of Dragonfly software to derive
silicon particles in the modified region (right side of the interface) quantitative information such as total
which have very low contrast in the absorption contrast mode. Image
on the right is a 3D multi-planar view representation showing the volume and size distribution of the
location of YZ and XY slices (not shown) in the 3D volume. A few silicon particles and voids, as shown
particles that remain unmodified are also seen on the far right sides in Fig. 5. The software also enables
of the images grouping and fragmented analysis of
the image data. The histogram tool
enables a user to efficiently select a
subset of particles based on certain
characteristics and perform analysis on
the chosen group.
Additionally, the integration of
the 3D visualization and quantitative
analysis module enable 3D rendering
of the overlaid quantified data. From
Figure 5 Results of the 3D Quantitative data analysis of the phase
contrast data from the Al-30Si sample. (a) 3D visualization of phase the 3D rendering and quantitative
contrast data (b) Surface rendering of segmented voids. (d) Volume data from histograms shown in Fig. 5
representation of all the silicon particles. it can be inferred that FSP effectively
3D visualization of 3D visualization of voids 3D visualization of quantified
phase contrast data particle data
a b c
S6 Tomography and image analysis March/April 2017 | MicroscopyandAnalysis
modifies the microstructure in the
alloy, reducing the large silicon pieces
to less than 5 µm.
The images also suggest that the
modified particles were uniformly
distributed in the FSP region with
no detectable agglomerations. An
additional result observed from
the analysis was the size and wide
distribution of voids seen in the base
alloy before modification. Voids are
known to lower the strength and
toughness of a material by heavily
contributing to the initiation and
propagation of cracks.
The FSP processed zone shows
a drastic reduction of the number
and size of the voids, which suggests
that the mechanical properties must
be significantly enhanced within
the analyzed volume. Additional
mechanical characterization tests
need to be carried out to ascertain this
observation and to link the property
enhancement to microstructure
modification through FSP. The
datasets contain rich morphological
information which could also aid
in qualitatively and quantitatively
assessing the particles in terms of shape
and roughness.
Previously only available at
synchrotrons, a new modality available
on the Zeiss 520 Xradia Versa is
Laboratory Diffraction Contrast
Tomography (LabDCT)5. LabDCT was
used to determine the crystallographic
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 3D MICROSTRUCTURE OF HYPEREUTETIC ALLOY

A b biography
A. Gourav Rao is a scientist and group
leader for the Friction Stir Welding
group at Naval Metallurgy Division,
Naval Materials Research Laboratory
(NMRL), Ambernath, India. He
graduated in metallurgical engineering
from Indian Institute of Metals and
was awarded a PhD from the Indian
Institute of Technology Bombay for his work on the
effect of friction stir processing on microstructure and
mechanical properties of Al-30Si alloy. He has many
years of experience studying the structure-property
correlation of metals and alloys using advanced
microscopy techniques and is author of twenty seven
peer-reviewed international journals with two patents
to his credit.
Hrishikesh Bale is an applications
specialist in the materials science
business sector at Carl Zeiss Microscopy,
LLC in Pleasanton CA, where he
works on applications development
of laboratory 3D X-ray imaging
techniques both at micro and nano-
scale. His research is focused on
diffraction contrast tomography and in-situ micro
and nano-mechanical testing while imaging using
X-ray computed tomography. His background is
Figure 6 LabDCT results from the Al-30Si sample. (a) Reconstructed LabDCT data from in mechanical engineering and materials science,
raw diffraction patterns (shown in b) from the sample in the cube plot representation. with many years experience in synchrotron X-ray
The cubes represent silicon grains in the sample; width represents the size of the grains,
and color represents the crystallographic orientation of the grains. Note the clustering
microscopy and tomography. He received his Ph.D.
of the cubes of the left hand side of the sample which is the unprocessed part of the from Oklahoma State University and worked as a post-
sample. After sample modification by FSP the silicon grains were reduced in size (<5 µm) doc at Lawrence Berkeley National Laboratory. He is
well below the LabDCT detectability limit. author of over 35 peer-reviewed scientific publications,
conference proceedings and technical presentations.

orientation of individual silicon
particles within the aluminum matrix.
LabDCT works by utilizing the X-ray
diffraction patterns collected from
the sample to determine the 3D
crystallographic orientation.6 Some
initial results from LabDCT imaging
on the Al-30Si sample are presented.
Detailed investigations of these results
are reserved for future studies.
The results from LabDCT revealed
the crystallographic orientations of
larger silicon particles as shown in
Fig. 6. The additional information of
crystallographic orientations of the
silicon phase helps in understanding
if there is a preferred orientationor
anisotropy of the dispersed silicon
grains, which could potentially be an
important processing parameters.
A detailed study to understand the
influence of crystal orientation on the
material properties is required since
such a non-destructive approach to
gather crystal information in these
materials has never been applied
before. However, LabDCT has been
applied to titanium (Ti-β21S) and
compared to EBSD and synchrotron
DCT7.
SUMMARY AND CONCLUSIONS
In this work, we have demonstrated
the use of non-destructive three
dimensional X-ray imaging to
investigate the microstructural
modifications obtained by FSP in
an Al-30Si composite. Despite the
low differences in the absorption
coefficients of aluminum and silicon,
the two phases were very clearly
discerned using the propagation
phase contrast mode. Quantitative
analysis of the particle and voids was
performed and resulting data shows
the effectiveness of FSP in modifying
the microstructure in order to improve
the mechanical properties of this
important class of contemporary high
performance structural materials.
REFERENCES
1 Mishra RS et al. Mater. Sci. Eng., A,
2003, 341, 307–310
2 Gan YX et al. Materials 2010, 3, 329-
350
3 Salih OS et al. Materials & Design Vol.
86, 5, 2015, 61–71.
4 Tewari A et al. Mater. Sci. Eng., A
2006, 428, 80–90.
5 http://www.theobjects.com/
dragonfly/index.html
6 C Holzner et al., Micros. Today, 24, 4,
p. 34–43 (2016).
7 SA, McDonald et al. Scientific Reports
5, 14665 (2015).
©John Wiley & Sons Ltd. 2017
abstract
Using 3D X-ray microscopy for microscale imaging,
we describe the results of a non-destructive study on
a two-phase hypereutectic aluminum silicon alloy
from a novel approach of friction stir processing (FSP).
A phase contrast imaging mode is used to discern
the microstructural refinement of the silicon particles
within the aluminum matrix along with the quantitative
data analysis that enables a full three-dimensional
analysis of the voids and particle distribution. Despite
the low differences in the absorption coefficients of
aluminum and silicon, the two phases were very clearly
discerned using the propagation phase contrast mode.
Quantitative analysis of the particle and voids was
performed and resulting data shows the effectiveness of
FSP in modifying the microstructure in order to improve
the mechanical properties of an aluminum-silicon
hypereutectic alloy.
acknowledgements
The authors would like to acknowledge Dr. S.B. Singh,
Outstanding Scientist & Director, NMRL, Ambernath for
his constant support and encouragement.
Corresponding author details
Dr. A. Gourav Rao, Naval Metallurgy Division, Naval
Materials Research Laboratory, Shil-Badlapur Road,
Addl. Ambernath (East)- 421506, Thane, India. +91-251-
2623174, Fax: +91-251-2623004, email: gourav@nmrl.
drdo.in
Dr. Hrishikesh Bale, Carl Zeiss X-ray Microscopy, 4385
Hopyard Rd, Pleasanton, CA 94588, USA. +1-925-701-
3534, email: hrishikesh.bale@zeiss.com
Microscopy and Analysis 31(2): S4-S7 (AM),
April 2017

MicroscopyandAnalysis | Tomography and image analysis March/April 2017 S7

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