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Three-Dimensional EBSD Characterization of Thermo-Mechanical Fatigue Crack Morphology in Compacted Graphite Iron
Three-Dimensional EBSD Characterization of Thermo-Mechanical Fatigue Crack Morphology in Compacted Graphite Iron
ScienceDirect
www.elsevier.com/locate/matchar
Article history: In cylinder heads made of compacted graphitic iron (CGI), heating and cooling cycles can
Received 25 July 2013 lead to localized cracking due to thermo-mechanical fatigue (TMF). To meticulously
Received in revised form characterize the complex crack path morphology of CGI under TMF condition, in relation
24 October 2013 to microstructural features and to find out how and by which mechanisms the cracks
Accepted 19 January 2014 predominantly develop, three-dimensional electron back scattering diffraction (EBSD) was
employed. Based on the precise quantitative microstructural analysis, it is found that
Keywords: graphite particles not only play a crucial role in the crack initiation, but also are of primary
Three-dimensional EBSD significance for crack propagation, i.e. crack growth is enhanced by the presence of graphite
Thermo-mechanical fatigue particles. Furthermore, the density of graphite particles on the fracture plane is more than
Crack path morphology double as high as in any other arbitrary plane of the structure. The obtained results did not
Compacted graphite iron indicate a particular crystallographic preference of fracture plane, i.e. the crystal plane
parallel to the fracture plane was nearly of random orientation.
© 2014 Elsevier Inc. All rights reserved.
⁎ Corresponding author at: Department of Metallurgy and Materials Science, Ghent University, Technologiepark 903, 9052 Gent, Belgium.
Tel.: + 32 9 331 04 49; fax: + 32 9 264 58 33.
E-mail addresses: Hadi.pirgazi@ugent.be (H. Pirgazi), s.ghodrat@tudelft.nl (S. Ghodrat), leo.kestens@ugent.be (L.A.I. Kestens).
1044-5803/$ – see front matter © 2014 Elsevier Inc. All rights reserved.
http://dx.doi.org/10.1016/j.matchar.2014.01.015
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provided with a circumferential notch in the middle of the with colloidal silica as abrasive particles) solution, with a
gauge length, with a depth of 0.2 mm and a 0.04 mm tip particle size of 0.04 μm. In this step an automatic polishing
radius (cf. Fig. 2). Cracks were always found to initiate from machine with a uniform rotational speed was used to make
graphite particles at or near the notch tip, and in this respect a sure that all sections are parallel to each other. Furthermore, the
possible influence of surface roughness on TMF lifetime (as plan paralellity of the individual layers was also controlled by a
would be the case when using a smooth specimen) can be series of micro-Vickers indentations around the measured area.
excluded when using notched specimen. The thickness of layers (Z distance) was measured using the
A high-frequency induction generator was used for same Vickers indentations and fixed to 8.0 ± 0.5 μm. This value
heating. Cooling was accomplished by blowing compressed is fine enough to cover all desired microstructural details of the
air from three sides onto the specimen and by thermal sample, and is big enough to make it possible to have a full 3D
conduction into the water-cooled specimen grips. Detailed microstructure in a reasonable time. In total 31 sections were
information about TMF test procedures and specimens is prepared to cover a total Z length of 240 μm. The EBSD
reported elsewhere [7,12,13]. measurements were carried out by employing a high resolution
The TMF test was performed under total constraint condi- FEI Quanta™ 450 FEG-SEM. EBSD patterns were obtained and
tions, meaning that the total strain measured by the extensom- analyzed by means of TSL® software. Each EBSD measurement
eter was kept constant. By cycling the temperature between was carried out in the middle of the gauge length of the TMF
50 °C and 420 °C, out-of-phase (OP) TMF loading was accom- loaded sample in an area of 6000 × 700 μm2. For each section
plished. Note that the applied constant temperature range two adjacent EBSD scans with dimensions of 3000 × 700 μm2
(50–420 °C) in combination with the coefficient of thermal were merged. These measurements were performed with an
expansion of the CGI (16 × 10−6 K−1) leads to a fixed mechanical in-plane step size of 3 μm on a square grid scanning pattern, by
strain range of almost 0.6%, indicating that cyclic plasticity is which the finest microstructural details of this material could
bound to occur and a limited amount of cycles to failure is most be detected.
probable. Holding times of 30 s were applied during both
maximum and minimum temperatures in order to stabilize
temperature levels throughout the specimen. This TMF test 3. Results and Discussion
procedure is intended to replicate the thermal and mechanical
conditions in the valve bridge area of cylinder heads. 3.1. Data Processing
2.3. Three-dimensional Measurements The first step to reconstruct the 3D microstructure is the
alignment of the sections. Different alignment algorithms
To have a better understanding of the effect of the crystallo- have been already proposed and the most important ones are
graphic orientation on the TMF crack growth path, a TMF loaded based on the maximization of mutual information of two
sample, with 195 cycles to failure, was investigated by 3D EBSD adjacent sections. In this study an algorithm, which is based
measurements using the manual serial sectioning technique. on the minimization of the average disorientation between
This method includes consecutive steps of sample preparation two adjacent sections was used [14]. The algorithm proposed
and EBSD measurements. The sample preparation consists of by Lee et al. [14] was improved by considering the rotational
mechanical polishing with OP-S (oxide polishing suspension displacement as well as X–Y displacement between the slices.
Fig. 2 – Circumferential notched dog-bone specimen with notch depth of 0.2 and a 0.04 mm tip radius. Dimensions are
indicated in mm. LD is loading direction.
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According to the method applied here, it was observed that for which defines the length d. Next, for two consecutive layers
a particular alignment of two sections, always a well defined the closest neighbor vertex points are determined, defining
minimum exists and this minimum is taken into account as the lengths d1 and d2 (cf. Fig. 3a). The shortest length d1 is
the correct alignment position. After alignment, a triangula- chosen to close the loop of the first triangle (cf. Fig. 3b). This
tion algorithm was employed to reconstruct the crack surface. procedure is repeated recurrently to expand the entire
To this purpose, an algorithm proposed by Saylor et al. [15] triangulation mesh (cf. Fig. 3c).
was used. The triangulation started from the notch tip Although the EBSD measurements provide extensive micro-
whereby points from two consecutive layers are connected structural information especially about the crystallographic
to each other according to the schedule shown in Fig. 3a, orientation, because of the low indexation rate in the vicinity of
the crack it was not possible to precisely determine the
morphology of the crack edge from the EBSD scans. For this
reason, in addition to the EBSD scans, high resolution secondary
electron SEM images were also recorded. For each section
several secondary electron images with a magnification of 700×
were collected through the entire surface and were merged to
show a high resolution large scale view of the surface (cf. Fig. 4).
As it can be seen from this figure crack and graphites were
separately highlighted with different colors using a MATLAB
image processing toolbox and some manual corrections. This
marking allows obtaining a sharp separation between metal
matrix, graphite particles and the crack. These SEM images
were converted to the format of an EBSD data set. For this
purpose, it was assumed that each pixel of the image is one
scan point with X and Y coordinates directly recovered from the
X and Y coordinates of the pixels of the SEM image and Euler
angles, image quality and confidence index arbitrarily assigned.
To distinguish between crack, graphite and metal matrix, they
were considered as three different phases. This helps us to look
at crack and graphite separately in the ParaView® software,
which is used for 3D image reconstruction.
Subsequently, the secondary electron derived data sets with
graphite and crack as two separate phases were merged with
the real EBSD scans. In order to do this, the scan information of
graphite and crack derived from the SEM images was substitut-
ed in the real EBSD scan. This produces a new file with three
phases (iron, crack and graphite) and the crystallographic
orientations of the iron phase. The inverse pole figure (IPF)
map of the reconstructed volume after applying the above
mentioned procedure is presented in Fig. 5.
Fig. 4 – (a) Secondary electron SEM image through the entire thickness; this image consists of several individual images. The
horizontal length of the image is 6 mm (crack is highlighted as blue and graphite as red). (b) The same image with higher
magnification (LD and RD are loading and radial directions, respectively).
The measured distribution of the ω angle together with the plane. It can be seen that the measured distribution of ω
random distribution is shown in Fig. 8. This random distribu- closely resembles the random distribution of ω. The average
tion represents the distribution of the angle between the values of ω for the measured and the random distributions are
normal of randomly distributed planes and the nearest {001} equal to 32.5° (with the standard deviation of 11.7°) and 36.5°,
respectively. This result shows that there is no preferred
crystal plane that is parallel to the crack plane and strongly
suggests that the brittle fracture in CGI does not occur on the
traditional {001} cleavage planes. This may be related to the
fact that the pearlite metal matrix does not represent a
continuous volume of BCC crystal, but a fine mixture of BCC
ferrite and orthorhombic cementite (Fe3C).
In order to check the hypothesis of crystal orientation
effect on the crack path, a further analysis was carried out. In
the previous evaluation it was found that there was no overall
influence of crystal orientation on the crack propagation. It
still remains to be verified, though, if the crystal orientation
might have a local effect far away from the graphite particles,
where there is no influence of the graphite morphology. To
this purpose, the value of ω was evaluated as a function of
distance to the nearest graphite particle in the crack plane and
determined in the 3D sample volume (cf. Fig. 9). If the crystal
Fig. 6 – Schematic drawing of the crack plane and a {001} orientation effect were to play a role far away from the
plane with ω angle. graphite particles, one would expect a negative slope of the
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Fig. 7 – Lateral view of the crack path exhibiting the ω angles according to the color code of the legend. The black regions
represent the graphite particles on the crack plane.
curve that represents the ω value versus the distance to the area fraction of graphite particles in the planes parallel to the
nearest graphite particle. The measured data derived from the crack path—excluding the crack path itself—(9.6%) implies
3D data set, however, do not show such a descending slope, that the graphite morphology is nearly isotropic (cf. Fig. 10).
but nearly a constant ω value (~32°) that very well approx- The present study, based on the precise quantitative
imates the average of the random distribution (~ 36°). microstructural analysis shows that graphite particles are of
primary significance for crack propagation. However, it
3.3. Graphite Particles Distribution remains to be determined by which interaction mechanism
the crack is guided through the metal matrix aiming for the
The data analysis suggests a crucial role of graphite particles maximum area fraction of graphite particles. In this respect,
in the crack propagation mechanism, as it appears that the two main mechanisms might play a role: (i) the stress
crack path jumps from one graphite particle to the neighbor- concentration field around a graphite particle interacts with
ing one (cf. Fig. 4) and crystal orientation is not of importance. the stress field at the crack tip, and (ii) a delaminated zone at
It was established that the total area fraction of the crack the graphite metal interface represents a small microcrack in
plane covered by graphite particles is equal to 23.9% (cf. Fig. 7). the bulk of the metal matrix equally exhibiting a local stress
However, this number has to be compared with the average distribution that will interact with the main crack. Consider-
fraction of graphite particles covered in arbitrary planes. 3D ing the observation of graphite delamination, which was
analysis shows that the average area fraction of graphite extensively observed here (cf. Fig. 11), the second hypothesis
particles for a number of more than 1000 arbitrary planes is appears to be more probable [12].
equal to 9.4% (with the standard deviation of 3.9%). Further- This finding may have important technological conse-
more, the comparison of the measured area fraction of quences. In CGI, the graphite particles are of a vermicular
graphite particles in the crack path (23.9%) with the average morphology randomly distributed in space. The present study
Fig. 8 – Measured and random distribution of ω angle as derived from 3D EBSD data.
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Fig. 10 – Distribution of graphite particles in (a) the crack plane, (b) an arbitrary plane parallel to the crack path and (c) an
arbitrary plane inclined to the crack plane.
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