Available online at www.sciencedirect.

com

ScienceDirect
Procedia Structural Integrity 7 (2017) 133–140
www.elsevier.com/locate/procedia

3rd International Symposium on Fatigue Design and Material Defects, FDMD 2017
19-22 September 2017, Lecco, Italy

Influence of post fabrication heat treatments on the fatigue behavior of

Ti-6Al-4V produced by selective laser melting
Gianni Nicoletto1, Stefania Maisano2*, Michele Antolotti2, Filippo Dall’Aglio1
1
University of Parma, Dept. of Engineering and Architecture, 43124 Parma, Italy
2
BEAM-IT srl, Strada Prinzera, Fornovo Taro – Italy

Abstract

Selective Laser Melting (SLM) is characterized by a layer-wise building process that enables the near net shape production of
parts with a high geometrical complexity. The SLM process leads to the build-up of thermal stresses, while the rapid
solidification leads to segregation phenomena and the development of non-equilibrium phases. To reduce thermal stresses and to
optimize the microstructure and the mechanical properties for the specific application, suitable post-production heat treatments
should be defined. Four different heat treatments in vacuum of SLM Ti6Al4V were investigated in relation to the fatigue
behavior. Tensile and fatigue specimens were produced with a SLM system using the optimized process parameters.
Microstructures before and after heat treatment were characterized by metallographic methods. Two post fabrication heat
treatments are promising in terms of fatigue strength of as-built SLM Ti6Al4V. The role of surface machining was also
investigated for one heat treatment condition.
Copyright © 2017 The Authors. Published by Elsevier B.V.
Peer-review under responsibility of the Scientific Committee of the 3rd International Symposium on Fatigue Design and Material Defects.
Keywords: Fatigue, Ti-6Al-4V, selective laser melting, heat treatments

* Corresponding author. Tel.: +39 0525 401281 ; fax: +39 0525 406949 .
E-mail address: s.maisano@beam-it.eu

2452-3216 Copyright  2017 The Authors. Published by Elsevier B.V.

Peer-review under responsibility of the Scientific Committee of the 3rd International Symposium on Fatigue Design and Material Defects.
10.1016/j.prostr.2017.11.070
13 Gianni Nicoletto et al. / Procedia Structural Integrity 7 (2017) 133–140

1. Introduction

Powder bed fusion (PBF) is one of the seven AM technologies identified by ASTM norm and it is mainly aimed
at producing parts using metal alloys such as Titanium, Ni-based super alloys, Cr-Co alloys and Al/Si alloys.
Alternative acronyms within the same technology are: SLM (selective laser melting), SLM (direct metal laser
sintering) where a laser is the energy source and EBM (electron beam melting) where the source is an electron beam,
see Bandyopadhyay and Bose (2016). In the rest of the paper the SLM acronym will be used to specify the key role
of the laser energy source on the powder bed process.
The Ti6Al4V alloy is the most widely used Ti alloy in high-value-added industrial sectors such as aerospace,
medical, energy, motorsport etc.. The SLM process, which is characterized by a layer-wise building process that
enables the near net shape production of parts with a high geometrical complexity, is recently complementing
traditional production routes of Ti parts, such forging and casting. The SLM process offers several additional
advantages compared to conventional production techniques, such as reduction of production steps, a high level of
flexibility and a high material consumption efficiency, see Srivatsan and Sudarshan (2016).
To industrialize the SLM process as well as to design and qualify the SLM part, the quality of processed material
has to be controlled and the mechanical properties determined and guaranteed. The SLM process is characterized by
the build-up of thermal stresses, while the rapid solidification activates segregation phenomena and the development
of non-equilibrium phases. Therefore, suitable post-production heat treatments should be defined to mitigate thermal
stresses and to optimize the microstructure and the mechanical properties for the specific application.
The influence of post fabrication heat treatments on static properties of SLM Ti6Al4V has been recently
investigated by different authors, for example Vranken et al. (2012), Rafi et al (2013). However, the fatigue
performance is often the critical design parameter for many high-value applications. Several investigations of the
fatigue characteristics of Ti6Al4V materials produced with layered AM techniques have been published recently.
Measured fatigue strength of as-built SLM Ti6Al4V was shown to be considerably lower than that of wrought,
annealed material, for example Leuders et al. (2013), Edwards and Ramulu (2015), Mower and Long (2016). The
influence of microstructural directionality on fatigue behavior of SLM Ti6Al4V was investigated by Bača et al
(2016). Since surface machining of SLM Ti6Al4V specimens improves the measured fatigue strengths approaching
corresponding conventional (wrought and machined) materials, the fatigue behavior in the presence of as-built
surface is especially important.
This contribution presents the results of a systematic investigation of the fatigue behavior of SLM Ti6Al4V in
dependence of four different post-fabrication heat treatments. Tensile and fatigue specimens were produced with a
state-of-the-art SLM system using optimized process parameters. Microstructures before and after heat treatment
were examined using metallographic methods. Since one of the major challenges of the SLM technology is the poor
fatigue behavior of its high roughness surfaces, the present fatigue tests were mainly performed using as-built
specimens, although the influence the machined surface was quantified in one case.

2. Experimental details

2.1. SLM fabrication

Ti6Al4V-ELI powder (Extra Low Interstitials) was used for specimen fabrication using an EOS M290 system
with a laser power of 400 W, a spot size of 100 m and a layer thickness 60 µm. The Ti6Al4V powder had a particle
size ranging from 15 to 45 m. The building platform was heated to 80°C during the job and the fabrication process
was in an Argon gas atmosphere. A large set of cylindrical tensile and fatigue specimens were produced with axis all
oriented in the build direction (i.e. axis Z). The laser motion in the individual layer was programmed on the base of a
contour and core strategy.

2.2. Post fabrication heat treatments

The as-built microstructure of SLM Ti6Al4V consists of a fine a circular martensite called α’ phase, see Vranken
et al (2012). The associated mechanical properties are high yield and ultimate strength, but a relatively low
ductility.
Post-fabrication heat treatments have been investigated to improve the ductility of Ti6Al4V products manufactured
by SLM and to achieve a variety of desired mechanical properties. Temperature of β-transus transformation is
critical in the heat treatment: heating below or above it influences the relative quantity of α and β phases, which
results in a lamellar morphology or in the development of columnar grains, Rafi et al (2013).
Four different post fabrication heat treatments were investigated in this study. Details are as follows:

HT 1 - 740°C for >1 hr, vacuum cooling to 530° C in >1 hr and cooling to room temperature in Ar.
HT 2 - 740°C for >1 hr and cooling to room temperature in Ar.
HT 3 - 1200°C for >1 hr, vacuum cooling to 530°C in >1hr and cooling to room temperature in Ar.
HT 4 - 900°C for > 1 hr, vacuum cooling to 530°C in >1 hr and cooling to room temperature in Ar
All these heat treatments are classified as Annealing HT. In particular, HT1 and HT2 are annealing treatments
below the β- transus temperature while HT3 and HT4 are above this temperature.

2.3. Metallographic preparation

Metallographic samples were cut from specimens with a K “Remet” SiC blade and cleaned with acetone in an
ultrasonic bath and dried with compressed air. Lapping operation with abrasive SiC papers from the coarsest grain
size to the finest one (i.e. 400, 800, 1200, 2000 mesh) was carried out before a final OPS polishing for 40 min.
Kroll’s etchant (6 ml HNO 3 ,2 ml HF, 92ml H2O) was used to reveal the Ti6Al4V microstructure. The optical
microscopy investigation and recording was performed on Zweiss Axio Observer system.

2.4. Mechanical tests\

Mechanical properties of the material such as ultimate strength, yield stress and elongation were characterized by
uni- axial tensile tests. Tensile specimens were machined from cylindrical bars of SLM Ti6Al4V according to the
ASTM F2924-E8 (M) standard geometry, see Fig. 1, where the length of reduced section A=30mm, reference
diameter D=6mm, gage length G=25mm, and fillet radius R= 6 mm.

Fig. 1 Tensile specimen geometry according to ASTM F2924-E8 (M)

Fig. 2 shows fatigue specimens with the two conditions of surface finish examined: as-built and machined. Key
geometrical parameters were: reference diameter D = 6 mm, total length L = 80mm, gripping diameter G = 12mm
and fillet radius R= 20 mm. The stress concentration factor was K t = 1.1 Fatigue tests were performed in fully
reversed, rotating bending mode at room temperature and with a frequency of 50 Hz on a multi-station fatigue
machine. Samples of each heat treated material were tested with stress amplitudes ranging from just below the yield
strength down to levels that produced lifetimes up to 10 7 cycles. Unbroken specimens after 107 cycles were removed
and termed “run- out”.

Fig. 2 Rotating bending specimens with the as-built and machined surfaces.
3. Results

3.1. Microstructures

Microstructures after heat treatment were investigated using metallographic methods and presented in Fig.3. The
microstructures shown in Fig. 3 are characterized by a lighter alpha phase and darker beta phase. In HT1 and HT2
samples the laser scanning path is visible even after the heat treatment, while in the other two samples this particular
feature is not observed.

Fig. 3 Microstructures of SLM Ti6Al4V after the four post fabrication heat treatments
a) HT1, b) HT2, c) HT3, d) HT4
The characteristic α lamellar morphology can be identified in almost the whole section of HT1 and HT2
specimens, (see Fig. 3a and 3b). In particular, islands of fine martensitic grains are identifiable in a complex
structural network, which is defined “Widmanstӓtten structure”, see Vranken et (2012). HT3 specimen of Fig. 3c
shows a remarkable grain coarsening due to the high temperature it has been subjected to during the heat treatment.
The α” lamellar microstructure(see Morri) can also be observed in this metallographic section. Finally, HT4 sample
of Fig. 3d is characterized by a homogeneous α microstructure, in which lamellar grains are slightly coarsened and
shorter in size if compared to the ones obtained after HT1 and HT2.The cooling rate is the most important parameter
that determines the phases and the morphology. Furnace cooling results in lamellar α+β and Argon cooling results in
“Widmanstӓtten
structure” and α’ martensite. The lamellar spacing and the alpha grain boundary thickness decrease with increase
cooling rate.

3.2. Tensile behavior

Tensile test results on the specimens subjected to the different post fabrication heat treatments are presented in Fig.
4. Ultimate tensile strength UTS and elongation at break E% are considered. Several observations can be made: i)
mechanical properties for all heat treated samples are above the specific minimum ASTM F2924-14 requirements
for additive manufactured Ti6Al4V, namely UTS= 895 MPa and E%= 10%; ii) the post fabrication heat treatments
influence mainly the elongation at break, which is an index of material ductility; iii) HT1 and HT2, which differ for
the cooling rate, show a similar ultimate strength but an improved elongation at break of the HT1 treatment; iv) HT3
data show the worst mechanical properties of the four heat treatments in terms of both strength and elongation; v)
HT4 specimens show high ultimate tensile strength and the maximum elongation at break.

a) b)
Fig. 4 Influence of post fabrication heat treatment on tensile properties of SLM Ti6Al4V
a) ultimate strength b) elongation at break

3.3. Fatigue behavior

The rotating bending fatigue tests performed to determine the influence of the post fabrication heat treatment are
presented in Fig. 5 and show that this influence is more significant than on static properties. In detail, the HT1
specimens show good fatigue properties with a low data scatter. As regard the heat treatment HT2, while the tensile
results were similar to HT1, the fatigue behavior is definitely worse than that of HT1 with remarkably shorter lives.
The HT3 treatment, which was characterized by the worst tensile results, shows a good high cycle fatigue behavior,
close to that obtained with the HT1 treatment. A good performance, both tensile and in fatigue, is determined with
HT4 specimens. It is pointed out that the run-outs at the highest stress amplitudes were associated to this HT4 heat
treatment but with a somewhat high scatter.
The influence of the as-built surface on fatigue was investigated on a set of specimens heat treated according to
HT1 and then machined on an automatic lathe. The comparison of the as-built and of the machined data is presented
in the fatigue plot of Fig. 6. An experimental as-built surface fatigue knock-down factor Cas-built = 0.3 is estimated
using the respective fatigue strengths at 107 cycles.
Although the roughness of the as-built SLM surface is the result of several mechanisms that are not discussed
here, it is reminded that the surfaces of a SLM part of complex geometry may be too expensive or even impossible to
machine. As an additional information, although the surface roughness of the present as-built rotating bending
specimens was not measured directly, as-built flat specimens produced under the same conditions and oriented in the
Z direction were characterized by an average roughness Ra= 13.4 m and Rz = 80.7 m, see Konečná et al (2017).
 Fig. 5 Influence of post fabrication heat treatment on fatigue behavior of heat treated and machined SLM
Ti6Al4V

MACHINED

AS BUILT

Fig. 6 Influence of surface machining on fatigue behavior of heat treated HT1 SLM Ti6Al4V

The present original fatigue results on SLM Ti6Al4V heat treated according to HT1 are now introduced in the
plot of Fig. 7 to discuss different sets of data found in the literature: i) fatigue data of Ti64 produced in an EOS
system and tested in rotating bending in the machined state after a HIP treatment, see Edwards and Ramulu (2014)
ii) fatigue data of Ti64 produced by conventional process (i.e. wrought) and polished, see Mower and Long (2016)
iii) scatter band of fatigue data for Ti64 produced conventionally but with different levels of surface finish, see
Lütjering et al (2007).
 Fig. 7 Comparison of present data on SLM Ti6Al4V and fatigue behavior of conventional Ti6Al4V.

Inspection of Fig. 7 shows that: i) the HIP process does not represent a source of improvement in the case of high
quality of the SLM process because internal defects on which HIP has a positive effect are very limited in number
and small (i.e. theoretical densities greater than 99.9 % are typical of an optimized SLM process on Ti6Al4V), ii) the
HT1 treatment of SLM Ti6Al4V and subsequent surface machining achieves a fatigue strength comparable to that of
conventionally produced Ti6Al4V, iii) the literature signals a sensitivity of the surface finish on the fatigue behavior
of conventional Ti6Al4V, which is expected to play a role even in SLM Ti6Al4V.
As a general comment on material defects and the SLM process, they may be internal, near-surface or surface-
breaking for example after machining. Internal defects can in principle be eliminated by a HIP treatment if oxides are
not present thus preventing surface welding. The high temperature of the HIP treatment results in reduced
mechanical properties compared to an optimized heat treatment (for example HT1). The as-built surface associated
to the SLM process is intrinsically rough. Such roughness, on which HIPing has no influence, can be interpreted in
terms of an equivalent surface defect to be used in fatigue life estimates according to damage tolerant approaches.

4. Conclusions

In this paper, the influence of four post fabrication heat treatments in a vacuum furnace of Ti6Al4V produced with
a state-of-the-art SLM system and process was investigated in terms of microstructure, tensile properties and fatigue
behavior. The comprehensive study demonstrates that two heat treatments, one above and one below the  transus,
are especially valuable for the associated high fatigue strength and tensile properties above the ASTM requirements.
Due to the practical importance of the as-built surface condition, the present fatigue tests were mainly performed
on as-built and heat treated specimens. For one heat treatment condition, the influence of surface machining was
quantified and allowed the definition of an as-built surface knock-down factor in fatigue of 0.3. This factor is high
but comparable to traditional process-affected (i.e. casting or forging) surface factors.
The present fatigue results for SLM Ti6Al4V demonstrated that this laser-based additive manufacturing process
achieves performances that are comparable to conventional processes when the surface conditions are similar.

References

ASTM F2924-14, Standard Specification for Additive Manufacturing Titanium-6 Aluminum-4 Vanadium with Powder Bed Fusion, ASTM
International, West Conshohocken, PA, www.astm.org (2014)
Bača A., R. Konečná, G. Nicoletto, L. Kunz, “Influence of build direction on the fatigue behaviour of Ti6Al4V alloy produced by direct metal laser
sintering”, Materials Today: Proceedings 3 921-924 (2016).
Bandyopadhyay, A., Bose, A. Additive manufacturing: Additive manufacturing technologies of metals using powder-based technology. Taylor &
Francis Group: Boca Raton (2016). 377 p.
Edwards P., Ramulu M. “Fatigue performance evaluation of selective laser melted Ti–6Al–4V” Mater. Sci. Eng. A, (2014), A598, 327–337
Konečná R., G. Nicoletto, S. Fintová, M. Frkáň, “As-built surface layer characterization and fatigue behavior of DMLS Ti6Al4V”, Proceedings
FMDM3, Lecco (2017), in press
Leuders L., M. Thöne, A. Riemer, T. Niendorf, T. Tröster, H. A. Richard, H. J. Maier, “On the mechanical behaviour of titanium alloy TiAl6V4
manufactured by selective laser melting: Fatigue resistance and crack growth performance”, Inter. Jou. Fatigue, 48, 300-307 (2013).
Lütjering G., Williams J.C., A. Gysler A., Microstructure and mechanical properties of titanium alloys. Titanium: Springer Science and Business
Media, (2007).
Morri A. “Trattamenti termici delle leghe di Titanio α+β, correlazioni fra microstruttura e comportamento meccanico” La metallurgia italiana,p.1-
9 (2008)
Mower T. M., M. J. Long, “Mechanical behavior of additive manufactured, powder-bed laser-fused materials”. Materials Science and Engineering,
A651 198-213 (2016).
Nicoletto G., “Anisotropic high cycle fatigue behavior of Ti-6Al-4V obtained by powder bed laser fusion”. International Journal of Fatigue,
(2016), vol. 94, pp. 255-262.
Rafi H. K., N. V. Karthik, H. Gong, T. L. Starr, B. E. Stucker, “Microstructures and mechanical properties of Ti6Al4V parts fabricated by selective
laser melting and electron beam melting”, Jou of Materials Engineering and Performance, 22, 3872-3883 (2013).
Srivatsan, T.S., Sudarshan, T.S. Additive manufacturing: Innovations, Advances and Applications. Taylor & Francis, Boca Raton, (2016). 444 p.
Vrancken B., Thijs L., Kruth J.P.,Van Humbeeck J., “Heat treatment of Ti6Al4V produced by Selective Laser Melting: Microstructure and
Mechanical properties”, Journal of Alloys and Compounds, (2012). 541(0): p. 177-185.