Powder Metallurgy

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Axial fatigue testing of Ti–6Al–4V using an

alternative specimen geometry fabricated by
metal injection moulding

J. Soyama, O. M. Ferri, T. Ebel & K. U. Kainer

To cite this article: J. Soyama, O. M. Ferri, T. Ebel & K. U. Kainer (2016) Axial fatigue testing of
Ti–6Al–4V using an alternative specimen geometry fabricated by metal injection moulding,
Powder Metallurgy, 59:5, 344-349, DOI: 10.1080/00325899.2016.1251060

To link to this article: https://doi.org/10.1080/00325899.2016.1251060

Published online: 08 Nov 2016.

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 Axial fatigue testing of Ti–6Al–4V using an
alternative specimen geometry fabricated by
metal injection moulding
J. Soyama∗ , O. M. Ferri, T. Ebel and K. U. Kainer
The hourglass-shaped specimen, which is commonly used for axial fatigue testing, cannot be
easily fabricated by metal injection moulding. Consequently, this work aimed at evaluating the
performance of an alternative specimen (dog bone geometry) for fatigue characterisation.
Additionally, an effort towards the assessment of the fatigue damage with specimens fatigued
until halflife was made. The alloy used in this study, serving as an example for the test
validation, was Ti–6Al–4V. The feasibility of using the specimens for fatigue testing was
confirmed with a narrow scatterband, however, only in the range of 105 cycles. The crack
initiation sites were always found on the surface associated with quasi cleavage facets.
Specimens fatigued until halflife showed a decrease in ductility in conventional tensile testing;
nonetheless, the ultimate tensile strength remained unchanged.
Keywords: Ti–6Al–4V, MIM, Axial fatigue testing

Introduction type of specimen is very hard to be fabricated by

Ti–6Al–4V presents attractive properties such as high
specific strength at room and moderate temperatures,
good corrosion resistance and biocompatibility.1,2 The
applications of Ti–6Al–4V, however, have some con-
straints related to raw material and processing costs.
Wrought alloys are the most commonly used; neverthe-
less, other processing routes that do not need extensive
machining and avoid material waste are gaining popu-
larity. One of the most prominent processes that allow
cost-effective near-net shape fabrication of complex geo-
metries corresponds to metal injection moulding (MIM).
It has been recently shown that MIM-processed tita-
nium alloys can achieve ultimate tensile strength
(UTS) of approximately 850 MPa and ductility of
around 14% with 3.5% of residual porosity.3–6 Addition-
ally, with a close control of the process, the overall
impurities and especially the oxygen level can be kept
sufficiently low.
Up to now, however, the fatigue behaviour of MIM
components in axial loading was only scarcely charac-
terised. The most common geometry for axial fatigue
testing corresponds to the hourglass shape, which has
a continuous radius between the grip ends with the mini-
mum diameter at the centre. To guarantee crack
initiation inside the gauge length, the cross-section of
the grips’ area should be at least four times that of the
test area, according to the ASTM E466 standard.7
Owing to the special geometrical requirements, this
Helmholtz-Zentrum Geesthacht, Institute of Materials Research, Max-
Planck-Straße 1, D-21502 Geesthacht, Germany
∗
Corresponding author, email julianosoyama@gmail.com
MIM without machining operations and consequently
loss of the as-sintered surface. Not only is the sample
integrity compromised because of the thinner cross-sec-
tion in the middle, but also is the concentricity affected
during sintering, which negatively influences the
measurements of fatigue properties. Therefore, the possi-
bility of using alternative specimen geometries, which
are easily produced and that have a representative as-
sintered surface, would widen the choices of tools for
fatigue characterisation of MIM components.
A significant characterisation effort, regarding the fati-
gue properties of MIM components, was carried out by
Ferri et al.3,8,9 using the smooth bar geometry in four-
point bending configuration. Niinomi et al.10 employed
flat specimens with a rectangular cross-section in axial
loading and achieved results in the same range. Recently,
Horke et al.11 reported fatigue measurements in a rotating
bending configuration using machined hourglass speci-
mens from MIM pre-forms. However, no related publi-
cation could be found, in which the common MIM dog
bone-shaped specimen was used for fatigue testing. In
comparison to bending, axial loading offers the advan-
tage of a larger volume of material under maximum
load in addition to a more homogeneous stress distri-
bution along the cross-section.
In this work, axial fatigue testing of Ti–6Al–4V was
conducted using dog bone-shaped specimens (ISO
2740). Fatigue tests were also stopped at halflife, and
the specimens were ultimately fractured by tensile test-
ing. Fractographic analyses were applied to find the
crack initiation sites and identify the fatigue initiating
defects, as well as measure the stable crack propagation
length.

© 2016 Institute of Materials, Minerals and Mining

Published by Taylor & Francis on behalf of the Institute
Received 29 September 2015; accepted 15 October 2016
344 DOI 10.1080/00325899.2016.1251060 Powder Metallurgy 2016 VOL 59 NO 5
 Soyama et al. Axial fatigue testing of Ti–6Al–4V using an alternative specimen geometry fabricated by MIM
Materials and experimental procedures
Ti–6Al–4V grade 23 pre-alloyed powder with particle size
<45 µm, produced by gas atomisation, was used to pre-
pare the specimens. The powder was supplied by TLS
Technik GmbH, Bitterfeld, Germany. The binder system
comprised paraffin wax, stearic acid and polyethylene
vinyl acetate. The preparation of the feedstock was done
at the ratio of 35 vol.-% of binder system to 65 vol.-%
of metallic powder.
Figure 1 shows the dog bone-shaped tensile specimens
according to ISO 2740 prepared by MIM. First, the feed-
stock was produced by mixing the metallic powder and
the binder system in a Z-blade mixer under argon atmos-
phere for 2 hours at 120°C. After pelletising, the feedstock
was injection moulded with an Arburg 320S machine. In
order to remove the paraffin wax component, a chemical
debinding was conducted in a bath of heptane at 40°C for
20 hours. Thermal debinding and sintering were con-
ducted in a single-step heat treatment run. Sintering was
carried out at 1400°C for 2 hours in high vacuum
(10−4 mbar).
Density measurements were carried out by the immer-
sion method. The theoretical density taken for compari-
son was measured on the specimens produced by MIM
from the same pre-alloyed powder under the same con-
ditions used in this study, which were additionally hot iso-
static pressed (HIPed) in order to eliminate the residual
porosity. The value obtained was 4.41 g cm−3. The poros-
ity was calculated by subtracting the specimen’s densifica-
tion (measured density divided by theoretical density)
from 100% (full dense condition). Additionally, the pore
size distribution was calculated with the aid of a software
for image analysis (Olympus Soft Imaging Solutions,
AnalySIS Pro, Olympus, Tokyo, Japan). Four pictures
were used in order to obtain a representative amount of
pores analysed. The contents of interstitial elements (O,
C and N) were measured using a conventional LECO
melt extraction system. The amount of nitrogen and oxy-
gen was determined using the TC – 436AR, while carbon
was quantified by the CS – 444.
In order to characterise the microstructure of Ti–6Al–
4V, an investigation using light microscopy was carried
out. Four dog bone-shaped specimens were initially cut
in representative regions of the cross-section. The pieces
were subsequently mounted, ground, polished and ulti-
mately etched for 7 seconds using Kroll’s reagent. The α
colony size measurement was performed with the aid of
the same image analysis system as mentioned before.
The principle used by the software was the intercept
method, as described by ASTM E112 standard.12 A series
of five straight lines were horizontally drawn on a picture,
and the number of colonies intercepted was counted. This
1 Dimensions in mm of a sintered dog bone-shaped tensile
specimen
number was then compared to the unit length of the test
line and as a result, the mean α colony size was deter-
mined. The determination of the limits of the colonies
(colony boundary) was done manually. In total, four
different pictures with the same magnification (200×)
were used.
Tensile and fatigue testing
Dog bone-shaped tensile specimens were used for fatigue
testing of Ti–6Al–4V. The experiments were carried out in
air at room temperature using a resonance machine fabri-
cated by RUMUL, Neuhausen am Rheinfall, Switzerland
(Mikrotron 654-H, 20 kN). The sinusoidal waveform was
applied under load control at a frequency of approxi-
mately 100 Hz. The stress ratio used was R = 0.2, which
means that the specimens were ideally subjected only to
axial tensile–tensile loads. The maximum load applied
was 400 MPa. Grips that were specially adapted for this
experiment are shown in Fig. 2.
In order to ensure that fatigue failure would happen
within the 30-mm gauge, the regions of the specimens in
contact with the grips were shot-peened by zirconia
spheres with a diameter of 500 µm. Shot-peening induces
residual compressive stress and also provides a better sur-
face quality, thus crack initiation should take place within
the as-sintered region. The fatigue tests were conducted in
a set of two experiments:
I Specimens loaded until fatigue failure.
II Specimens loaded until the halflife of the previous
experiment.
The first experiment (I) focused on determining the fati-
gue life with the testing conditions applied (400 MPa of
maximum loading and R = 0.2), whereas the second
experiment (II) was used for the evaluation of microstruc-
tural damage at halflife. The specimens from the second
experiment (II) were thus pulled in a tensile test machine
to induce final fracture. Consequently, a picture of the
fatigue damage at 50% of life was evaluated by tensile
testing. This procedure is valid considering that, once fati-
gue damage is introduced, the specimen should rupture
right at the place of the propagated crack (weakest
spot). The measured stress–strain curves for fatigue
damaged and normal conditions were then compared. A
servo hydraulic machine Zwick 050 with a load capacity
of 50 kN was used for the tensile tests. The tensile tests
were carried out in air at room temperature with a strain
rate of 1.2 × 10−5 s−1. The testpieces had their 30 mm
gauge length attached to a mechanical extensometer.
Fractography investigations were conducted using the
scanning electron microscope DSM962 from Zeiss in all
fracture surfaces obtained. The recorded images were sub-
sequently used to find the fatigue crack initiation sites by
closely examining the outer area of the fracture surfaces.
Fatigue crack initiation sites in Ti–6Al–4V usually show
specific microstructural features (the quasi cleavage
2 Grips used to hold the dog bone-shaped tensile specimen
Powder Metallurgy 2016 VOL 59 NO 5 345
Soyama et al. Axial fatigue testing of Ti–6Al–4V using an alternative specimen geometry fabricated by MIM
3 Statistical data of porosity for Ti–6Al–4V sintered at 1400°C for 2 hours in vacuum: a pore size distribution; b form factor of the
pores
facets)13,14 that help uncover their location. The fatigue
crack propagation length was measured by the image
analysis based on the morphology of the different areas
between stable (smooth) and unstable (dimple-like)
crack propagation. The starting point was always the fati-
gue initiation site after which the smooth area (stable
crack propagation) followed.
Results and discussion
Porosity, interstitial elements and
microstructure
Table 1 displays the sintered density of the MIM pro-
cessed Ti–6Al–4V. Clearly, a high densification was
achieved, indicating that the sintering parameters applied
were adequate for this alloy. Porosities in this range were
also reported previously.3,8 Additionally, Fig. 3 shows the
statistical data of porosity for sintered Ti–6Al–4V, con-
firming that sintering was successful. The pore size distri-
bution was relatively fine with about 90% of the pores
containing sizes below 300 µm2 (Fig. 3a). The majority
of the pores were also round with at least 60% showing
form factor close to 1 (Fig. 3b).
Table 2 shows the amount of interstitial elements (O, C
and N). The analysed pieces were cut from different
regions of one tensile specimen. Each value was averaged
from three measurements. Since the starting powder cor-
responded to an extra low interstitial (ELI, grade 23)
with interstitial oxygen around 1000 µg g−1, the oxygen
pick-up was approximately 1000 µg g−1, whereas the car-
bon and nitrogen contents were within the range of the
grade 23 alloy. Considering that a high-sintering tempera-
ture was used (1400°C), the sintering atmosphere was suf-
ficiently clean to prevent extensive pick-up of interstitials
elements. These interstitial levels are also at the same
order of magnitude from previous works.3,8
Figure 4 shows a micrograph of the MIM processed Ti–
6Al–4V alloy. The microstructure consists of pores (dark
roundish areas) and large α colonies with an average
Table 1 Density measurement and the porosity of Ti–6Al–4V
prepared by MIM
Sintered density/g cm−3 Porosity/% Densification/%
4.26 3.32 96.7
346 Powder Metallurgy 2016 VOL 59 NO 5
size of 128 ± 13 µm. The colonies consist of laths of α tita-
nium with ribs of β titanium arranged in a coarse lamellar
pattern. The round shape of the porosity indicates that
sintering got to its final stage. However, owing to the
high temperature used in the process (1400°C), the α colo-
nies were significantly larger than observed in previous
studies,3,8 in which sintering was conducted at 1250°C
leading to α colony size in the range of 90–100 µm.
Mechanical properties and fractography
analysis
Table 3 shows the amount of cycles to failure of the speci-
mens that were subjected to fatigue testing. At the con-
ditions applied, the defined endurance limit for high-
cycle fatigue of 107 could not be reached. The results,
however, display a narrow scatterband for the moderate
lifetime of 105 cycles. The crack propagation length before
final failure was on average 1839 µm corresponding to
almost half of the specimen’s diameter.
The results of the first experiment (I) demonstrated the
feasibility of using tensile specimens for fatigue testing in
an axial tension–tension configuration. Nonetheless, this
was proved only for fatigue lifetime of 105 cycles. The
low performance of the tensile specimens at higher cycles
was due to the friction between the grips and the clamped
specimen, which caused fretting fatigue and induced fail-
ure outside the test area.
Niinomi et al.10 obtained lifetimes of 105 cycles at a
maximum stress of 500 MPa with Ti–6Al–4V, thus
100 MPa higher than the value measured in this work.
A possible explanation corresponds to the significantly
smaller specimens used by Niinomi et al., which led to a
smaller volume tested under cyclic loading. The surface
quality had supposedly only a minor influence, consider-
ing that the specimens from Niinomi were also tested in
the as-sintered condition and with similar colony sizes.
Ferri et al.3 obtained a similar result (105 cycles at
500 MPa) with four-point bending using smooth bar
Table 2 Contents of interstitial elements from the powder
and sintered piece
Element O/µg g−1 C/µg g−1 N/µg g−1
Starting powder (max.) 1300 800 500
Sintered piece 1917 ± 30 577 ± 13 147 ± 9
 Soyama et al. Axial fatigue testing of Ti–6Al–4V using an alternative specimen geometry fabricated by MIM

4 Sintered microstructure of MIM processed Ti–6Al–4V

Table 3 Specimens tested until fatigue failure

5 Fracture surface of a fatigue-failed specimen. The line deli-
Cycles to Crack propagation mits the stable crack propagation area
Specimen failure (105) length/µm

1 1.98 1871 previous experiment. There is no scatter in these values,

2 0.84 1821 because the test was manually stopped. The crack propa-
3 1.07 1861 gation length was significantly smaller than before with an
4 1.17 1804 average value of 304 µm.
Mean value 1.3 ± 0.5 1839 ± 32 Figure 6a shows a typical fracture surface from second
The maximum stress was 400 MPa, R = 0.2. experiment (II), in which the specimens were ultimately
fractured by tensile testing. It is possible to identify the
specimens of Ti–6Al–4V in the as-sintered condition. The crack initiation site and the stable crack propagation
lower value measured with the dog bone-shaped speci- area, which was significantly smaller than from first
mens could be attributed to the larger volume under fati- experiment (I). Figure 6b corresponds to a picture of
gue and the different configuration of the fatigue test crack initiation site, whereas Fig. 6c shows, in higher mag-
(axial loading). On the other hand, Horke et al.11 reported nification, the fatigue initiating defect. The fatigue initiat-
very similar values to the ones presented in this paper. At ing defects could be easily identified by the fracture
400 MPa, the amount of cycles to failure was in the order surface analysis. These defects were always found at the
of 105 cycles using the rotating bending configuration. surface of the specimens associated with quasi cleavage
Figure 5 shows a representative fracture surface of Ti– facets that represent a typical sign of fatigue crack
6Al–4V from the first experiment (I), in which rupture initiation in Ti–6Al–4V. The facets result from the separ-
took place by fatigue failure. The fracture surface in ation of intense slip bands under the action of a tensile
Fig. 5 confirms that failure really occurred due to fatigue stress normal to the plane of slip.13 When a favourably
since a region of stable crack propagation is clearly distin- oriented grain is stressed, the dislocations glide until
guished, which extends almost until the middle of the they meet a grain boundary causing a pile-up, leading
specimen’s cross-section. The crack initiation site (indi- to facet formation.
cated by a white arrow) is followed by a large stable It is widely accepted that for high-strength materials
crack propagation area on the left-hand side, which when low oscillating loads are applied (high-cycle fatigue
extends almost until the middle of the specimen. This regime), the most critical contribution corresponds to the
region is characteristically flatter than the final fracture fatigue initiation, which could take as much as 90% of the
area that consists mainly of dimples (right-hand side). fatigue life.15 Considering such premise, if this condition
Table 4 shows the number of cycles of the specimens would hold in the case of the material tested, the speci-
that were fatigued until the halflife measured in the mens loaded until the halflife should not show any sign
of fatigue cracks. Nonetheless, that was not the case, as
can be seen in Fig. 6. Not only crack initiation took
place, but also a small stable crack propagation area
Table 4 Specimens tested until the fatigue halflife could be identified (the smooth area on the fracture
Number of Crack propagation
Specimen cycles (105) length/µm Table 5 Mechanical properties of Ti–6Al–4V in different
conditions
1 0.65 206
2 0.66 235 YS/ UTS/
4 0.66 394 Condition MPa MPa Elongation/%
5 0.65 380
Mean value 0.66 304 ± 97 Reference (undamaged) 744 ± 5 852 ± 2 14.7 ± 0.7
Fatigue damaged until 753 ± 6 858 ± 2 11.1 ± 3.7
The maximum stress was 400 MPa, R = 0.2.
halflife

Powder Metallurgy 2016 VOL 59 NO 5 347

Soyama et al. Axial fatigue testing of Ti–6Al–4V using an alternative specimen geometry fabricated by MIM
6 A characteristic fracture surface of a specimen fatigue tested until the halflife. Final fracture was caused by tensile testing: a
fracture surface of the specimen’s cross-section displaying a small stable crack propagation area; b the crack initiation site; c
detail of the fatigue initiating defect and the quasi cleavage facet
surface). In fact, Fig. 6 actually depicts a situation where
crack initiation and propagation took place because the
length involved is large (around 400 µm). Instead, if
only crack initiation would have taken place, this length
should be in the order of magnitude of the microconstitu-
ents, e.g. α colony size, corresponding to a microstructu-
rally short crack. The fast crack initiation process could
be attributed to fatigue testing with the as-sintered surface
that contains many irregularities. As reported by Ferri
7 Typical tensile test curves of as-sintered Ti–6Al–4V and
fatigued until halflife
348 Powder Metallurgy 2016 VOL 59 NO 5
et al.,8 the fatigue endurance limit can be significantly
improved by modifying the as-sintered surface with
shot-peening.
In contrast to the replica technique16 in which an image
of the surface is imprinted in a tape or the direct obser-
vation of the specimens’ surface on the microscope,17
the post-mortem fractographic observation of fatigue
crack initiation provides the advantage of examining the
crack length inside the specimen. Additionally, it allows
tensile testing of fatigued specimens, which can be used
to roughly assess the fatigue damage. Figure 7 shows
the typical stress–strain curves obtained by tensile testing
of an undamaged and a fatigue-damaged specimen.
Clearly, there is a decrease in ductility of about 4% in
the fatigue-damaged specimen; however, the shape of
the tensile curve remained unchanged.
Despite the decreased ductility of the fatigue-damaged
specimens, the yield strength (YS) and UTS remained the
same, as shown in Table 5. Considering that the fatigue
crack at 50% of fatigue life was, on average, about
300 µm, the results show that the Ti–6Al–4V alloy pro-
cessed by MIM is quite damage-tolerant under tensile
loading.
Conclusions
(i) Axial fatigue testing in tensile–tensile configur-
ation using a common dog bone-shaped speci-
mens prepared by MIM is feasible; however, the
 Soyama et al. Axial fatigue testing of Ti–6Al–4V using an alternative specimen geometry fabricated by MIM
defined endurance limit for high-cycle fatigue
could not be reached with these specimens due
to fatigue fretting at the contact with the grips.
(ii) Fractography analysis of the surfaces revealed the
fatigue initiating defects at the as-sintered surface,
as well as a region of stable crack propagation.
(iii) Specimens subjected to fatigue until the halflife
contained cracks in the order of 300 µm, which
decreased the ductility measured by tensile testing
but did not change the UTS.
Acknowledgements
The authors thank all those that actively contributed to
the realisation of this work: Andreas Dobernowsky,
Dirk Matthiessen, Hamdi Tek, Dr Jan Bohlen, Jürgen
Knaack, Manfred Horstmann, Petra Fischer, Wolfgang
Limberg, Uwe Lorenz and Dr Uwe Zerbst.
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