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Materials Science & Engineering A: Sciencedirect
Materials Science & Engineering A: Sciencedirect
Materials Science & Engineering A: Sciencedirect
A R T I C LE I N FO A B S T R A C T
Keywords: Finishing methods of additive manufactured metal parts are becoming a key driver of industrial viability, in-
Surface finishing creasingly with additive processes being challenged in demanding end-product applications. The same scenario
Ti alloys stresses the requirements as to fatigue life of parts built by Additive Manufacturing (AsM).
Fatigue life The paper addresses fatigue life of Ti6Al4V produced by Powder Bed Fusion in four finishing conditions: as-
Additive manufacturing
built, tool machined, after tumbling and after tumbling and subsequent shot-peening. Failure mechanisms at the
X-ray diffraction
Electron microscopy
micro-scale are observed in order to reinforce the mechanical results by identifying the role of different surface
morphologies in crack initiation. X-ray diffraction (XRD), scanning electron microscopy (SEM) techniques and
microanalysis (EDX) are used to investigate microstructural modifications generated by the different finishing
methods.
Results show that tumbling alone does not improve fatigue life against the as built condition, whereas
tumbling and subsequent shot peening allow matching the fatigue endurance of tool machined specimens. The
shot peening process causes surface amorphization and implantation of the peening media turning into sub-
surface inclusions. Based on the results, an optimized finishing process can be envisaged, consisting in prolonged
tumbling up to the removal of a stock allowance at least equal to the powder size, before shot peening.
1. Introduction Titanium alloys are certainly the most used and extensively in-
vestigated, as their construction by layer manufacturing immediately
Powder Bed Fusion (PBF) is an additive manufacturing process turned out as a strategic business opportunity. It is not surprising,
which is increasingly driving attention of political and research com- therefore, that ASTM F2924 (Specification for AM Titanium-6
munities, as its application fields are spreading at a rate that has no Aluminum-4 Vanadium with Powder Bed Fusion) came out in 2012 as
equal in western countries. PBF is opening new technological oppor- the first answer to standardization needs common to the additive
tunities for high-end products because of its huge technological ad- manufacturing (AM) industry [3,4]. It represents a clear attempt to
vantages, such as design ground-breaking freedom, allowing extremely bring some order, define a shared practice, and provide accountability
lightweight components with novel and integrated functionalities, fast tools, to the field of PBF. All these needs cannot be postponed if PBF
production without tooling finishing, high flexibility, and no costs for claims to emerge as competitive industrial process.
tooling investment [1]. In prosthetic and medical fields, as well as in aerospace, additive
It is a shared opinion that the rushed diffusion requires joint effort processes using Ti6Al4V find full capitalization of their distinctive
of scientific community to understand, control, standardize materials features, chiefly compliance to complex geometries, low volumes and
and processes to mitigate risks (and costs) of such an industrial re- strong individualization [5]. In addition to specific product categories,
volution. A qualitative leap is required in understanding and control a noteworthy field of success for PBF is the manufacturing of parts-on-
micro-mechanisms that often compromise long-term reliability of demand, with great logistic ease [6,7]. In aircraft industry many players
components. In order to meet the automotive, aerospace and defence are considering AM as an opportunity to reduce warehousing and
requirements more efforts are needed from the research side. Airworthy produce spare parts at time and place they are needed. For PBF tech-
PBF components require a thorough knowledge of the mechanical be- niques, aerospace is just a market as big as the implants and prostheses
havior, static as well as dynamic [2]. one.
∗
Corresponding author.
E-mail address: p.mengucci@univpm.it (P. Mengucci).
https://doi.org/10.1016/j.msea.2019.03.119
Received 4 March 2019; Received in revised form 27 March 2019; Accepted 28 March 2019
Available online 01 April 2019
0921-5093/ © 2019 Elsevier B.V. All rights reserved.
L. Denti, et al. Materials Science & Engineering A 755 (2019) 1–9
Recently, PBF technology has accomplished the goal of mechanical 2.2. Surface finishing processes
properties often equal to, or even better than those obtained by tradi-
tional processes [8]. Conversely, concerns are moving to part relia- In order to evaluate influence of post-processed surface finishing
bility, focusing research efforts on fatigue life studies as well as on risk treatments on mechanical properties, four different sets of samples were
factors capable of cutting them down [6]. In general, AM generates produced, namely: Tool Machined (TM), As Built (AB), Tumbled (T),
highly distinctive microstructure, totally dissimilar from that observed Tumbled and Shot-peened (TS).
elsewhere [9,10], that turns into an urgent need for better knowledge of Tool machined (TM) specimens were turned with cutting speed of
expected performances. Difficulties in predicting part characteristics to 20 m/min, feed rate 0.07 mm/rev.
ensure robustness and repeatability are still major limitations. The As Built (AB) set of samples, not submitted to any surface fin-
The success of AM is strictly connected to the possibility of trans- ishing treatment, is the reference condition.
lating complex and new shapes into real products. The proper manu- The Tumbling process (T) was carried out by standard procedure for
facturing of Ti-based components produced by the AM technique titanium alloys with ceramic media. A set of samples (named TS)
usually need specific design and optimization, because AM focuses on among the Tumbled (T) treated specimens was submitted to shot-pe-
customized parts or low volume production [11,12]. ening by using corundum (Al2O3) particles (size in the range
The mechanical performances of Ti-based parts produced by AM are 70 μm–140 μm) in compressed air at ∼ 50 psi (∼340 kPa) for 30 s.
strongly affected by thermal history and material properties [13,14].
Thermal effects are of particular relevance in AM because the technique 2.3. Roughness measurement
involves local rapid heating and cooling cycles that lead to skin effect
and development of unexpected microstructure in the final product Surface roughness was measured in accordance to DIN EN ISO
[15]. Furthermore, high temperature gradients and high cooling rate 4287/4288 and DIN EN ISO 25178. A Nikon LV 150 Confovis
induce thermal stresses, segregation phenomena and formation of non- Microscope was used to assess the surface topography with the fol-
equilibrium phases. The non-equilibrium phenomena depend on laser lowing configuration:
parameters, material properties and environmental conditions [16–18].
The mechanical behavior of parts produced by additive manu- • 20× microscopic objective;
facturing techniques have been extensively studied [19–22], and a • 0.595 μm lateral resolution, 10 nm vertical quantization and auto-
number of authors have investigated methods to improve the fatigue matic field stitching;
life of final products [23,24]. Moreover, influence of post-processing • 500 × 1200 μm scanned area.
2
and finishing processes on fatigue life has been also deeply investigated
[25–28]. Several papers have demonstrated that post-processing treat- A FALS filter (according to ISO 16610–62), cut off 8 μm × 8 μm, and
ments are capable of greatly improving mechanical performances as bilateral symmetric threshold filtering (for the removal of spikes) were
well as fatigue life of additively manufactured products, mainly attri- applied to the maps for form removal.
buting this effect to internal defects [29] and surface roughness The 3D average surface roughness (Sa) was calculated on the maps.
[30–32]. Surface homogeneity was checked in advance to validate the operation.
The present paper reports on the mechanical behavior of Ti6Al4V Sa provides a comprehensive measurement of the surface morphology.
alloy with α+β microstructure produced by powder bed fusion (PBF) Surface Skewness (Ssk) and Surface Kurtosis (Sku) was also calculated.
and post-processed by different surface finishing treatments. Fatigue Ssk describes the asymmetry of peaks/valleys to the median plane. At
life of as built (AS), tumbled (T), tumbled plus shot peened (TS) samples Ssk = 0, surface peaks and valleys are symmetrically distributed. With
have been compared to study the structural mechanisms responsible of Ssk < 0 valleys are predominant, while Ssk > 0 indicates surface pre-
the improved mechanical properties. Results have shown that the fa- ferentially formed of peaks. Sku is associated to the peak/valley
tigue behavior of alloy is independent on surface roughness, while sharpness. High Sku values (> 3) are typical of very sharp peaks. The
being strongly influenced by the post-production finishing treatment. Abbott-Firestone curve obtained from roughness measurements allows
The combined tumbling and shot peening processes increase up to identifying peak height (Spk) and valley depth (Svk) at the same time.
150% the value of infinite fatigue life maximum force of the material.
This effect is discussed in terms of surface amorphization and defects 2.4. Tensile and fatigue testing
reduction induced by the shot peening treatment.
According to UNI EN 6892-1 standard tensile tests have been per-
formed on cylindrical specimens, dimeter 4 m, gauge length 25 mm.
2. Material and methods Details of sample geometry for tensile tests are shown in Fig. 1a. An
Instron 5567 machine equipped with 30 kN load cell and extensometer
2.1. Material production and properties Instron 2630, gauge length 25 mm, was used for tensile tests. Test speed
was set at 2 mm/min.
Samples for tensile and fatigue tests were built from EOS Titanium Axial fatigue tests with constant amplitude (origin, R = 0) were
Ti64 (EOS GmbH - Electro Optical Systems) powder by using EOS M270 performed according to UNI EN 3987: 2010 (Aerospace Series - Metal
machine operated with standard parameters: laser scan speed Test Methods - High Fatigue Test with Constant Amplitude Force
1250 mm/s, laser power 340 W, hatch distance 0.12 mm, layer thick- Application) considering infinite lifetime limit 6·106 cycles. The S-N
ness 30 μm. All specimens were built along Z axis, i.e. parallel to the curves were obtained following UNI EN 3987: 2010 procedure speci-
growth direction. Nominal compositional range (wt.%) of Ti64 powder fications for stress increments/diminutions. Schematics of samples for
provided by manufacturer is reported in Table 1. axial fatigue tests are shown in Fig. 1b.
Before testing, tensile specimens were tool machined, while fatigue
specimens were tested in the different surface finishing conditions.
Table 1
After fatigue tests the fracture surface of samples was observed by
Nominal powder composition (wt.%). scanning electron microscopy (SEM).
Al V Ti O Fe C
2.5. XRD and SEM characterization
5.50–6.75 3.50–4.50 Bal. 0.2 max 0.30 max 0.08 max
Structural characterization of samples with different surface
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L. Denti, et al. Materials Science & Engineering A 755 (2019) 1–9
Fig. 1. Geometry and size of tensile a) and axial fatigue test b) specimens (unit: mm).
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L. Denti, et al. Materials Science & Engineering A 755 (2019) 1–9
Table 2
Experimental full width at half maximum (FWHM) values obtained from peak analysis of XRD patterns at gauge measured in the reduced angular range
(2θ = 34°–43°). Experimental values at shoulder of reference sample AB (column “Shoulder”) are reported for comparison.
Miller indices AB T TS Shoulder
2θ (deg) FWHM (deg) 2θ (deg) FWHM (deg) 2θ (deg) FWHM (deg) 2θ (deg) FWHM (deg)
(10-10) 35.34 ± 0.02 0.42 ± 0.06 35.380 ± 0.009 0.23 ± 0.03 35.14 ± 0.03 0.48 ± 0.09 35.279 ± 0.004 0.22 ± 0.01
(0002) 38.426 ± 0.007 0.20 ± 0.02 38.45 ± 0.01 0.24 ± 0.03 38.45 ± 0.01 0.46 ± 0.03 38.447 ± 0.002 0.268 ± 0.007
(10–11) 40.402 ± 0.002 0.193 ± 0.005 40.435 ± 0.002 0.219 ± 0.005 40.253 ± 0.006 0.55 ± 0.02 40.3581 ± 0.0006 0.253 ± 0.002
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L. Denti, et al. Materials Science & Engineering A 755 (2019) 1–9
Fig. 4. SEM images of specimen gauge section: a) AB, b) T, c) TS, d) TS at higher magnification with corundum (Al2O3) particles evidenced by arrows.
EDX analysis in spot mode on the spherical-shaped particle evidenced Dynamic fatigue tests show that T does not reach infinite life even at
high concentration of Al and substantial increase of oxygen, not con- 200 MPa, rather it breaks under 106 cycles. On the contrary, AB and TS
sistent with material composition. Therefore, the Al-rich particles im- reach infinite life at 200 MPa and 500 MPa, respectively. TM reaches
planted in the surface of sample TS has an external origin, due to the infinite life at 500 MPa. From these results one can conclude that TS
shot-peening media, that is corundum (Al2O3). increases infinite fatigue life maximum stress of about 150% against the
Material removal by the tumbling treatment followed by subsequent reference AB, resulting similar to TM. However, above 500 MPa TM
surface amorphization of the shot-peening process strongly influence shows higher fatigue cycle values (> 106 cycles) than TS.
surface morphology and crystallography of TS, reducing porosity and Fracture analysis by SEM observation was performed on AB, T and
lack of fusion defects (LOF), that are the typical initiating defects for TS samples broken after few fatigue cycles (about 104) to check possible
crack growth and propagation in additively manufactured parts [34]. presence of inner defects responsible of early break. On the contrary,
Quantitative results of roughness measurements are shown in for the TM condition, only broken samples at infinite life were ob-
Table 3, while roughness maps are reported in Fig. 5. served.
As evidenced in Table 3, Sa varies with surface treatment from Fig. 7 reports fracture surfaces of samples. All images show the
Sa = 21.5 μm for AB to 4.83 μm for TS. Values obtained for AB are crack start spreading point, and different cracking mechanisms can be
considered as reference. The tumbling (T) process slightly decreases Sa, identified.
changes skewness (Ssk) from positive to negative and decreases Kur- Fracture surfaces of TM in Fig. 7a and b shows rupture starting in
tosis (Sku). The TS process strongly decreases Sa and Ssk, and increases correspondence of a hole or melting failure, which is a weaker point.
Sku. The tool machined (TM) specimen, as expected, has very low In the machining process the tool machine removes surface layers
surface roughness (low values of Sa, Spk and Svk in Table 3) and ne- down to the bulk, so reducing or eliminating surface cracks. This action
gative Ssk. makes the fatigue failure mechanism of TM different from the other
Fig. 5 show roughness maps of samples where the turning action in samples, justifying the maximum stress at infinite fatigue life similar to
TM is recognisable as well as the finishing action of corresponding post- TS and the results of dynamic fatigue test at higher stress values
production process for T and TS samples when compared to the re- (Fig. 6).
ference (AB). In AB (Fig. 7c and d), T (Fig. 7e and f) and TS (Fig. 7g and h)
Results of the static tensile tests performed according to the UNI EN samples, no peculiar defects such as holes or material contamination
6892-1 standard are reported in Table 4, while results of dynamic fa- are visible, fracture takes origin from a surface microcrack.
tigue test are summarised in Table 5 and Fig. 6. The tumbling process (T) simply cuts powder particles adhered to
Tensile tests (Table 4) evidenced static mechanical behavior of the the surface, without any removing action of cracks on bulk surface.
investigated material in complete agreement with literature data for However, vibrations during the tumbling process tend to enlarge the
additively manufactured Ti64 alloy. unremoved surface cracks, giving rise to maximum stress at infinite life
lower than TS.
In Fig. 7h (TS) the SEM image shows a darker area near the surface.
Table 3 EDX analysis of the dark area provided an Al2O3 (corundum) compo-
Results of roughness measurements. sition. This further confirms that Al2O3 particles, used as abrasive in the
TM AB T TS shot peening process, tend to implant on the sample surface during the
surface treatment, preferentially filling empty spaces between bulk and
Sa [μm] 0.227 21.5 18.9 4.83
partially melted powder particles adhered to the surface, that were not
Ssk −0.255 0.553 −0.414 −1.6
Sku 2.70 2.81 1.94 5.69 completely removed by the tumbling treatment.
Spk [μm] 0.115 9.76 6.37 1.76 Shot-peening process modifies material surface giving rise to higher
Svk [μm] 0.227 11.9 9.99 3.28 fatigue resistance. However, it is not able to change mechanisms of
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L. Denti, et al. Materials Science & Engineering A 755 (2019) 1–9
crack initiation and propagation, that are identical to those observed in identical mechanism of crack initiation and propagation although their
AB and T samples. surface crystallography and roughness are deeply different. However,
Mechanisms responsible of fatigue failure involve initiating defects, TS sample shows a marked higher fatigue resistance respect all other
typically porosity and LOF, as well as crack growth and propagation samples. Bagehorn et al. [35] report improvement in the fatigue per-
[34,35]. Results obtained on AB, T and TS samples showed substantial formances of blasted Ti64 produced by additive manufacturing, mostly
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L. Denti, et al. Materials Science & Engineering A 755 (2019) 1–9
Table 4 a) reduces the number of defects on sample surface, that are responsible
Results of static tensile tests performed according to the UNI EN 6892-1 stan- of crack initiation and b) produces surface amorphization, that hinders
dard. crack propagation along preferential crystallographic directions.
Average value S. D. Double action of the shot-peening process causes marked improvements
in the fatigue behavior of additively manufactured samples.
UTS[MPa] 1170 24
Rp0.2% [MPa] 1122 32
εb [%] 10.9 1.4
4. Conclusions
E [GPa] 121 8
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