1 s2.0 S0921509324007524 Main
1 s2.0 S0921509324007524 Main
A R T I C L E I N F O A B S T R A C T
Keywords: Powder bed fusion (PBF), including selective laser melting and electron beam melting, fabricates complex,
Fatigue porous, osseointegrative implants for widespread clinical use. Fatigue testing is imperative for predicting long-
CoCr term strength and durability of rough and surface porous implants while bone remodels around and grows into
Ti6Al4V
the implant. This study analyzes different materials (Ti6Al4V and Co28Cr6Mo) with varying topographies
Powder bed fusion
Post-processing
including as-printed surface roughness and the addition of a surface porous layer common to implants. The
results are compared to wrought and PBF controls that are polished and machined. Moreover, different PBF
techniques for titanium result in different as-printed surface roughness (~0.07–17 μm) and microstructure. The
fatigue data demonstrates that the surface finish impact was stronger in Ti6Al4V versus CoCr and SLM Ti6Al4V
HIP + surface porous gyroid samples didn’t perform worse than the roughest solid sample without surface
porosity (EBM Ti6Al4V). With the same mechanical surface finishes, the SLM and wrought Ti6Al4V samples
display similar fatigue resistance (800 and 850 MPa respectively), while EBM samples remain inferior (350 MPa).
This study provides a foundation to compare fatigue resistance across materials and surface topographies
through different fabrication techniques to optimize the lifespan of orthopedic implants while incorporating
rough as printed surfaces and added surface porosity, both of which are essential for osseointegration.
1. Introduction modes, defects (i.e., porosity or surface roughness that behave as micro
notches) are inherent stress concentrations that act as crack initiation
Additive manufacturing (AM), specifically powder bed fusion (PBF), sites for fatigue failure [4]. Therefore, cyclic fatigue testing is imperative
has grown in popularity across multiple fields including the biomedical to predict the durability of implants over time. Other factors affecting
field for metallic orthopedic implants [1]. This process excels in pro fatigue life include cyclic stresses, residual stresses (from additive
ducing customizable, precise, and complex metal lattices (such as the manufacturing techniques), material properties (strength and tough
triply periodic minimal surface (TPMS) gyroid). These lattices, specif ness), internal defects, microstructure, surface quality, surface porosity,
ically the gyroid, are beneficial for promoting osseointegration in part oxidation, corrosion, etc. [5–7]. For high cycle fatigue (typically 100,
due to the superior mechanical properties compared to strut-based lat 000+ cycles), many cracks initiate at the surface defects, whereas in
tices [2]. In contrast, subtractive manufacturing, such as machining, very high cycle fatigue (typically 10 million + cycles) the cracks tend to
remains a useful technique for solid implants where patient specificity, initiate at internal defects [8]. Research has been conducted on the
porosity and surface roughness are not needed such as in standardized factors contributing to surface finish and minimizing internal defects
bone plates. While there are tradeoffs to consider with both 3D printing such as choice of material, type of manufacturing, optimizing
and machining, depending on the application, subtractive manufacturing process parameters, thermal post-processing for material
manufacturing can also be implemented with PBF to leverage the internal structure, and mechanical post-processing material external
strengths of both processes for certain device geometries [3]. finish (machining, polishing, blasting) [9–13]. However, especially
In orthopedic implants that undergo repetitive and complex loading when comparing across studies, past research efforts typically do not
Abbreviations: AM, additive manufacturing; PBF, powder bed fusion; TPMS, triply periodic minimal surface; HIP, hot isostatic pressing; SLM, selective laser
melting; EBM, electron beam melting.
* Corresponding author.
E-mail address: [email protected] (A. Heimbrook).
https://doi.org/10.1016/j.msea.2024.146821
Received 4 January 2024; Received in revised form 29 February 2024; Accepted 11 June 2024
Available online 13 June 2024
0921-5093/© 2024 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
A. Heimbrook and K. Gall Materials Science & Engineering A 909 (2024) 146821
Table 1
Summary Table for various properties of the tested samples.
Sample Name Post-processing Microstructure Surface Area Fatigue
Roughness (Sa) Strength
SLM Ti6Al4V HIP HIP 1650 ◦ F ± 25 ◦ F @ 14,750 psi +250/- elongated α in a lamellar α+β dual phase; 8.114 μm 325 MPa
246 for 2 h Widmanstätten morphology
SLM Ti6Al4V HIP + blasted HIP 1650 ◦ F ± 25 ◦ F @ 14,750 psi +250/- 5.141 μm 375 MPa
246 for 2 h
+ blasted
SLM Ti6Al4V HIP + machined HIP 1650 ◦ F ± 25 ◦ F @ 14,750 psi +250/- 0.203 μm 875 MPa
246 for 2 h + machined
SLM Ti6Al4V HIP + polished HIP 1650 ◦ F ± 25 ◦ F @ 14,750 psi +250/- 0.070 μm 800 MPa
246 for 2 h + polished
EBM Ti6Al4V As built Fine lamellar α+β dual phase; basket weave 17.24 μm 175 MPa
morphology
EBM Ti6Al4V + polished As built + polished 0.109 μm 350 MPa
wrought Ti6Al4V + machined Annealed @ 1300 ◦ F for 2 h + machined equiaxed α with dual phase lamellar α + β 0.238 μm 850 MPa
(transformed in between β)
wrought Ti6Al4V + machined Annealed @ 1300 ◦ F for 2 h + machined + 0.081 μm 850 MPa
+ polished polished
SLM Co28Cr6Mo Stress relief heat treated precipitates formed at grain boundary and within the 5.252 μm 375 MPa
1925 ◦ F ± 25 ◦ F for 2 h grains, predominantly γ
SLM Co28Cr6Mo + machined Stress relief heat treated @ 1925 ◦ F ± 25 ◦ F 0.197 μm 600 MPa
for 2 h
+ machined
SLM Co28Cr6Mo + polished Stress relief heat treated @ 1925 ◦ F ± 25 ◦ F 0.191 μm 525 MPa
for 2 h + polished
SLM Ti6Al4V HIP + 0.25 mm HIP 1650 ◦ F ± 25 ◦ F @ 14,750 psi +250/- N/A 200 MPa
gyroid 246 for 2 h
SLM Ti6Al4V HIP + 0.5 mm HIP 1650 ◦ F ± 25 ◦ F @ 14,750 psi +250/- N/A 150 MPa
gyroid 246 for 2 h
SLM Ti6Al4V HIP + 0.75 mm HIP 1650 ◦ F ± 25 ◦ F @ 14,750 psi +250/- N/A 175 MPa
gyroid 246 for 2 h
employ the same fatigue testing controls, samples, or methods across all residual stress and therefore improve resistance to crack initiation [27].
key permutations of the critical surface and processing variables. In EBM, on the other hand, requires a preheated temperature (which acts
particular, the addition of surface porosity compared to the as printed as an in-process heat treatment), and has less of a temperature gradient
rough surface has not been systematically analyzed in light of both during cooling resulting in less stress buildup and warping for the
printed and wrought, machined and polished controls. as-printed parts [6]. When comparing fatigue strength amongst PBF
Common metals implemented in orthopedic implants include processes, Vayssette et al., concluded that both SLM Ti6Al4V HIP and
Ti6Al4V and CoCr (specifically Co28Cr6Mo) due to their biocompati EBM HIP Ti6Al4V parts display a lamellar microstructure, yet, the
bility, corrosion resistance, and superior mechanical properties [1,14, roughness of the EBM parts caused a twofold decrease of fatigue stress at
15]. In PBF, these metals can be melted either through a laser source runout (222.5 MPa for SLM HIP and ~111.2 MPa for EBM HIP at 2
(Selective Laser Melting, SLM) or an electron source (Electron Beam million cycles in fully reversed loading) [28].
Melting, EBM) [16,17]. Different processing parameters alter the energy Surface post-processing alters material external finish by eliminating
density and will impact the quality of the manufactured part [18,19]. surface defects with machining, polishing, or powder blasting but
Moreover, when the molten metal cools in PBF, surrounding powder will cannot be practically applied to complex lattice PBF parts. These surface
adhere, which adds to the inherent surface roughness of a sample and post-processing techniques can be done individually or in addition to
lowers the fatigue properties in the as-built surface finish condition [20, thermal post-processing. Compared to Ti6Al4V samples with rough as-
21]. While most mechanical properties are lowered due to a rough built surfaces, machined samples typically have fatigue cracks initi
as-printed surface, the roughness enhances osseointegration leading to ating from either surface discontinuities or internal defects, whereas as-
an inherent tradeoff in the impact of surface roughness and porosity built samples with rough surfaces almost always experience crack
[22]. The wrought Ti6Al4V counterparts (made by deformation pro initiation at the samples surface [29]. Moreover, machining (removing
cessing and shaping the material in the solid state and then heat treating surface roughness) improves fatigue life, and machining on top of HIP
it) are almost always machined down to their final shape, so there is less further increased the fatigue strength [29,30]. Polishing can also mini
inherent surface roughness compared to as-built PBF surfaces. mize cyclic stressors (i.e., minimize stress concentrations to enhance
3D printed and wrought manufactured parts often receive thermal fatigue) with processes such as mechanical polishing, chemical polish
post-processing to minimize defects and favorably alter the micro ing, electro polishing, laser polishing, or a combination of the sorts
structure of the material. Thermal post-processing can include stress [31–35]. After mechanically polishing a SLM part’s surface, there can be
relief, heat treatment and hot isostatic pressing (HIP) all of which can improved monotonic tensile strength and fatigue strength due lower
alter the final microstructure and therefore mechanical properties [23]. roughness and compressive residual stress induced at the surface [36].
HIP applies high temperatures and pressure to decrease the internal For SLM Ti6Al4V samples in tested in tensile fatigue by Jamshidi et al.,
voids caused by processing and will in turn increase the mechanical the as-printed samples had a fatigue strength of ~50 MPa at 10 million
strength and fatigue life [24,25]. In one study, SLM CoCr as built sam cycles, but increased to ~200 MPa after HIP, and further increased to
ples had a fatigue strength of 135 MPa at 2 million cycles, which ~300 MPa with HIP and wet polishing [37].
increased to 319 MPa with HIP, and further improved to 380 MPa with Although research on individual factors influencing fatigue has been
heat treatment, with all variations displaying changes in microstructure published, there is a need to systematically compare multiple surface
and ratio of phases [26]. Moreover, the SLM process can produce re topographies under identical testing conditions and using an appro
sidual stresses from the temperature gradients due to fast cooling rates. priate fatigue sample geometry. It is widely known that increased sur
Thermal treatments are common for SLM parts as they help minimize face roughness lowers fatigue strength, yet there is little to no
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A. Heimbrook and K. Gall Materials Science & Engineering A 909 (2024) 146821
Fig. 1. Test set up of A) representative tensile samples after post-processing and with different surface porous gyroid samples (measurements in mm) and tensile test
set up B) representative high cycle fatigue samples after post-processing and with different surface porous gyroid samples (measurements in mm) as well as HCF test
set up.
information on how the deliberate addition of surface porosity impacts surface of the solid SLM TI6Al4V HIP parts) impacts the fatigue strength.
fatigue strength relative to as printed roughness and smooth wrought The gyroid is analyzed as it allows for bone to grow in, however the
and 3D printed controls. The current study encompasses testing different addition of the lattice introduces intentional defects where stress can
materials (Ti6Al4V and Co28Cr6Mo), various manufacturing techniques concentrate and lower the mechanical properties compared to the solid
(wrought, 3D printed by SLM, and 3D printed by EBM), and different counterpart. Ultimately, this work provides a foundational and sys
surface finishes (porous, as-printed, blasted, machined, and polished) to tematic study of the impact of multiple surface topographies on fatigue
better understand the influence of these variables on both monotonic properties of 3D printed metals (using common process and post pro
mechanical properties and fatigue behavior. The cylindrical dogbones cessing techniques documented in literature) relative to wrought Tita
tested under stress-controlled tensile high cycle fatigue (HCF) include nium material counterparts. The fatigue data is one essential component
the following solid sample groups: SLM Ti6Al4V HIP (as-printed surface, in understanding how to design and alter the surface of 3D printed im
blasted surface, machined surface, polished surface); EBM Ti6Al4V (as- plants to maintain fatigue resistance while still offering opportunity for
printed surface and polished surface) wrought Ti6Al4V (machined sur enhanced osseointegration.
face, machined + polished surface); SLM Co28Cr6Mo (as-printed sur
face, machined surface, and polished surface). Additionally, this study
establishes how the intentional addition of surface porosity (0.25 mm,
0.50 mm, 0.75 mm layer thickness of 65 % porous gyroid onto the
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A. Heimbrook and K. Gall Materials Science & Engineering A 909 (2024) 146821
Fig. 2. SEM images and roughness measurements (rounded to the hundredths) of the surface of A) SLM Ti6Al4V HIP variations B) EBM Ti6Al4V variations C)
wrought Ti6Al4V variations D) SLM Co28Cr6Mo variations E) SLM Ti6AlV HIP + gyroid.
2. Material and methods parameters (part LT30 in 3DXpert). For the gyroid lattice, refined infill
parameters were used (145 W laser power, 1000 mm/s scanning speed,
2.1. Manufacturing and thermal post-processing and 50 μm laser focus) [38].
All SLM Ti6Al4V parts (including surface gyroid parts) underwent
An overview of the sample names, manufacturing and post- hot isostatic pressing (HIP) at 1650 ◦ F ± 25 ◦ F at 14,750 psi +250/-246
processing methods can be found in Table 1. All 3D printed parts were for 2 h in accordance with ASTM 2924 -14. The samples were removed
designed in Solidworks. For both tensile and fatigue samples there were from the build plate via wire electronic discharge machining (EDM).
two variations: a dogbone with round ends and a cylindrical bar that The Co28Cr6Mo samples were printed in an inert Argon atmosphere
would be machined down to a dogbone (Fig. 1). For the SLM Ti6Al4V using a 3D Systems DMP ProX 350 system with 3DSystems CoCr F75
parts, 0.25 mm, 0.50 mm, and 0.75 mm of gyroid was added to the powder (15–53 μm particle size). Laser parameters of 250 W laser power
surface of the designed dogbone part during printing (Fig. 1). The gyroid and 1000 mm/s scanning speed were used for a single contour scan and
had a 6x6x6 unit cell size and 0.75 mm wall thickness and was applied infill. All SLM Co28CrMo parts underwent stress relief annealing at 1925
using 3DXpert. Parts were printed within a validated section of the build ± 25 ◦ F for 2 h. The samples were removed from the build plate with a
plate in the same direction of loading (tensile). wire EDM.
The SLM Ti6Al4V samples and SLM Ti6Al4V gyroid parts were The EBM Ti6Al4V samples were printed using a Arcam Q10plus V2.1
printed in an inert Argon atmosphere (3D Systems, DMP ProX 320; DMP machine with Ti–6Al–4V feedstock powder (45–146 μm particle size
ProX 350 for blasted samples) using grade 23 ELI Ti6Al4V feedstock distribution). The layer thickness was 50 μm, acceleration voltage was
powder 15–45 μm particle size distribution (AP&C) and default laser 60 kV and max beam current varied throughout the process but had a
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A. Heimbrook and K. Gall Materials Science & Engineering A 909 (2024) 146821
maximum of 50 mA. No further heat treatment was used. After printing, 2.4. Roughness measurements
samples were mechanically removed from the plate during cooling with
no additional tools required. All roughness measurements were taken on a Filmetrics Profilometer
The wrought Ti6Al4V (deformation processed and annealed) sam Standard with a 100 mm × 100 mm stage under 10× Nikon DI objective
ples were Grade 5 bars in accordance with ASTM B348 from Titanium lens with a zoom of 4x using white light interferometry. Three mea
Processing Center. The annealing took place at 1300 ◦ F for 2 h. The stock surements were taken of different parts of the gauge section of the
bars for tensile samples were 15.875 mm diameter and 78.74 mm long representative tensile sample.
and the stock fatigue samples were 15.875 mm in diameter and 88.9 mm
long. 2.5. Microstructure
2.2. Mechanical surface post-processing Micrographs were prepared based on the cross-sectional area of the
sample. Samples were cut by a water-cooled abrasive blade, then
All samples were threaded tensile or fatigue dogbones in accordance cleaned with ethanol and acetone and pressure mounted. From there,
with ASTM E8 and ASTM E466. The cylindrical wrought, SLM Ti6Al4V, the sample was ground with silicon carbide abrasives and polished with
and SLM CoCr samples were machined down to a dogbone shape with a diamond suspension and fine polished with colloidal silica (ASTM E3).
threaded ends. A set of samples from the SLM Ti6Al4V HIP, SLM Titanium samples were micro etched with Kroll’s reagent and Co–Cr
Co28Cr6Mo, EBM Ti6Al4V, and Wrought Ti6Al4V were polished from samples were etched with ASTM 20, per ASTM E 407.
the as built dogbone shape using increasingly fine grit paper in a process Optical microscopes (Leica DMI500) captured the micrographs at
standard in the polishing of total joints for articulation. Polishing by 500x, per ASTM E 883.
hand occurred until the desired mirror finish was reached. The wrought
Ti6Al4V samples were the only samples that received machining before 2.6. Mechanical testing
polishing. A group of SLM Ti6Al4V HIP samples were blasted with
Ti6Al4V particles ranging from 15 to 45 μm. Tensile and fatigue tests were based on ASTM E8 (tensile) and E466
(fatigue) samples and test protocols. All mechanical tests were on an
2.3. Surface SEM images MTS Landmark servo hydraulic test system. The samples were threaded
into custom made jigs (hardened stainless steel). Tensile tests (n = 4)
All SEM images were captured using an Apreo S by ThermoFisher were performed at a rate of 1 mm/min and fatigue testing was per
Scientific (formerly FEI) using a voltage of 2.00 kV and current of 25 pA. formed at a frequency of 10 Hz and R = 0.1 with n = 2 at each stress
Images shown are using the Everhart – Thronley Detector (EDS) using level. Tensile fatigue tests at 10 Hz were chosen to represent the worst
secondary electrons at a working distance of around 7 mm. case scenario of loading. Sample runout was defined as n = 2 reaching 1
million cycles at a given stress level. The jig was held into vee notch
grips at a pressure of 1250–1500 psi. The stress was calculated using the
cross-sectional area of only the base solid region for each sample,
Fig. 3. Micrographs of a representative sample in the A) SLM Ti6Al4V HIP B) EBM Ti6Al4V as-printed C) wrought Ti6al4V and D) SLM Co28Cr6Mo
manufacturing groups.
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A. Heimbrook and K. Gall Materials Science & Engineering A 909 (2024) 146821
Fig. 4. Static tensile stress strain curves of A) SLM Ti6Al4V HIP variations B) EBM Ti6Al4V variations C) wrought Ti6Al4V variations D) SLM Co28Cr6Mo variations
and E) SLM Ti6Al4V HIP + gyroid variations.
including the porous gyroid samples. from solidified melt pools as well as adhered unmelted particles. These
are both characteristic of the PBF process due to the laser/electron beam
2.7. Fracture analysis path, melting/solidification, and thermal diffusion. The EBM Ti6Al4V
samples have a larger particle size distribution (necessary for this
Optical images were obtained with an AM scope FMA050 with a fabrication method) compared to SLM Ti6Al4V HIP and thus appear to
LED-144. SEM images were taken using the same parameters as have larger solidified melt pools and larger particles adhered to the
mentioned in Surface SEM Images. surface. The combination of the two factors doubles the surface rough
ness of the EBM Ti6Al4V parts compared to the SLM Ti6Al4V HIP parts
3. Results and discussion (approximately 17 μm vs 8 μm). The SLM Co28Cr6Mo samples display
fewer and smaller adhered unmelted particles compared to both EBM
3.1. Surface analysis (roughness) Ti6Al4V and SLM Ti6Al4V HIP samples, which decreased the roughness
of the SLM Co28Cr6Mo sample to 5 μm. There are not as distinguishable
The average surface area roughness measurements (arithmetic mean solidified melt pools in the SLM Co28Cr6Mo samples which also
height, Sa) are quantified in Table 1 and Supplementary Table 1 along contribute to the smoother surface.
with SEM images of the surfaces which can be found in Fig. 2. Within The SLM Ti6Al4V HIP + blasted sample has far fewer adhered
each sample group (i.e., SLM Ti6Al4V HIP, Wrought Ti6Al4V, EBM unmelted particles and this powder blasting processing revealed more of
Ti6Al4V, and SLM Co28Cr6Mo), the mechanical post-processing greatly the solidified melt pools. Titanium powder blasting reduced the surface
reduces the surface roughness of the sample. roughness to about 5 μm which is about two-thirds the roughness of the
The surface of pre-mechanical post-processed PBF parts (SLM SLM Ti6Al4V HIP parts and approximately the same roughness as the
Ti6Al4V HIP, EBM Ti6Al4V and SLM Co28Cr6Mo) display roughness SLM Co28Cr6Mo sample. Independent of the material and method of
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A. Heimbrook and K. Gall Materials Science & Engineering A 909 (2024) 146821
3.2. Microstructure
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A. Heimbrook and K. Gall Materials Science & Engineering A 909 (2024) 146821
Fig. 6. Tensile behavior of A) ultimate tensile strength vs yield stress B) yield stress vs strain at failure C) ultimate tensile strength vs strain at failure.
surface porous SLM Ti6Al4V HIP + gyroid samples display a lower strain strength (Fig. 6A) and yield strength vs strain at failure (Fig. 6B), the
to failure compared to laser surface finishes (Fig. 4a) but comparable to Ti6Al4V and Co28Cr6Mo both display separate positive curved trends.
the strain to failure of the rougher EBM Ti6Al4V samples (Fig. 4b). For example, as yield increases so does the ultimate tensile stress. This
Of the solid Ti6Al4V samples, mechanical post-processing of the remains true for the Co28Cr6Mo samples with regards to yield strength
samples generally increases the average peak stress and yield strength, and strain at failure. However, the Ti6Al4V splits up into two separate
but there isn’t a distinct trend with strain at failure. While the wrought trends based on process (Fig. 6B and C) when strength is plotted against
samples have the highest average peak stress and average yield strength, strain to failure with the SLM Ti6Al4V HIP + gyroid and EBM Ti6Al4V
the SLM Ti6Al4V HIP and SLM Ti6Al4V HIP + blasted samples have the samples being grouped together at lower strain to failure levels vs the
largest average strain at failure indicative of a metallurgical difference SLM Ti6Al4V HIP and wrought Ti6Al4V samples grouped together at
in the 3D printed and wrought samples given how rough the 3D printed higher strain to failure levels. When the strain at failure increases, the
samples are. EBM Ti6Al4V samples show lower strain to failure while yield strength and ultimate tensile strength tend to decrease for the Ti
the SLM Ti6Al4V samples show more ductility similar to the wrought samples, but they do so at different rates for the SLM Ti6Al4V HIP +
samples. gyroid and EBM Ti6Al4V samples vs the SLM Ti6Al4V HIP and wrought
Amongst the gyroid SLM Ti6Al4V HIP samples, average peak stress Ti6Al4V samples. In both Fig. 6B and C, the SLM Co28Cr6Mo samples
and yield stress increases, and the strain at failure decreases, with more have a positive correlation compared to the Ti6Al4V samples. When
added surface gyroid (from 0.25 mm to 0.75 mm gyroid). Overall, the plotting ultimate tensile strength vs strain at failure (Fig. 6C), the
average peak stress and yield stress of the gyroid samples is higher than Ti6Al4V and Co28Cr6Mo overall become more cohesive which could
the solid counterpart in SLM Ti6Al4V HIP, but the strain at failure is indicate that for surface roughness treatments, as the ultimate tensile
lower. This is due to the extra porous gyroid aiding in strength since the strength increases so does the strain at failure. Since strain at failure is
stress was calculated using the cross-sectional area of only the base solid indicative of ductility, having a strong sample that is also ductile can be
region (i.e., 6.35 mm diameter instead of 6.85 mm, 7.35 mm or 7.85 mm a factor in determining fatigue life as local plasticity at notches and
diameters with the gyroid). However, the interface of the gyroid and stress concentrations can impact the nucleation of fatigue cracks.
solid acts as a stress concentration point causing lower strain to failure.
These surface porous gyroid parts display a lower strain fracture closer
to the EBM samples most likely due to the surface defects (roughness and 3.4. Fatigue behavior
porosity).
For the CoCr samples, the SLM Co28Cr6Mo + machined sample Fatigue behavior between different materials (Ti6Al4V and
displayed the highest peak and yield stress as well as the highest strain at Co28Cr6Mo), processes (wrought vs SLM and EBM), mechanical surface
failure. Since machining and polishing refined the surface roughness, post-processing (powder blasted, machined, and polished) and added
the strain at failure increased for a more ductile fracture. surface porous gyroid lattice (0.25 mm, 0.50 mm, and 0.75 mm) is
There are some correlations between certain tensile mechanical overviewed in Fig. 7 and summarized in Table 1 (see Supplementary
properties (Fig. 6). When plotting ultimate tensile strength vs yield Table 2 for more data). For each sample group, two individual samples
were tested at systematically decreasing levels of maximum applied
Fig. 7. Fatigue curves (maximum applied stress vs cycles to failure) of all sample variations.
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A. Heimbrook and K. Gall Materials Science & Engineering A 909 (2024) 146821
Fig. 8. Fatigue curves (maximum applied stress vs cycles to failure) of A) SLM Ti6Al4V HIP variations B) wrought Ti6Al4V variations and C) SLM Co28Cr6Mo
variations and D) SLM Ti6Al4V HIP + gyroid variations.
stress until sample failure occurred, or runout hit one million cycles. The both machined and polished are similar to each other.
data in Fig. 7 will be separated and discussed based on the key sample Blasting with Ti powder on the other hand (decreasing the surface
variables for clarity. roughness by ~36 %) only increases the fatigue life by 15 %. The slight
increase can be attributed to the decreased amount of adhered unmelted
3.4.1. Surface finish effect Ti6Al4V metal particles to the surface, but undercovering the presence
The effect of surface finish on fatigue life is conveyed in Fig. 8 when of undulations caused by solidified melt pools which act as stress con
each sample is grouped based on processing method and material (SLM centrations and potential fatigue crack nucleation sites. The SLM
Ti6Al4V HIP, Wrought TI6Al4V, EBM Ti6Al4V and SLM Co28Cr6Mo). Ti6Al4V HIP and SLM Ti6Al4V HIP + blasted samples started off having
The SLM Ti6Al4V HIP + surface gyroid samples were grouped with the a very similar fatigue life at higher maximum applied stresses, which
roughest samples that were produced by EBM. In general, within the further indicate how a slight change in surface roughness impacts high
same process group (i.e., SLM Ti6Al4V HIP, Wrought Ti6Al4V, SLM cycle fatigue versus low cycle fatigue which is expected. For the wrought
Co28Cr6Mo, and EBM Ti6Al4V with SLM Ti6Al4V HIP + gyroid sam samples, polishing the machined sample yielded only modest improve
ples), the smoother the surface, the better the fatigue life of the sample. ment in surface finish (machined samples are 3x rougher than polished),
This can be explained by the surface roughness acting as micro notches yet had minimal impact on fatigue strength at runout to 1 million cycles
on the surface for cracks to initiate due to the stress concentration. When (Fig. 8B). This suggests after a critical surface roughness of about 0.2 μm,
the surface roughness increases, the size of the micro notches also in further decreases in roughness are relatively ineffective in altering fa
creases and therefore less force is required for the cracks to initiate. tigue properties.
For the SLM Ti6Al4V HIP samples (Fig. 8A), machining the sample For the SLM Co28Cr6Mo samples (Fig. 8C), machining increases the
(decreasing surface roughness about 40x) increases the fatigue strength fatigue life by 60 % whereas polishing the sample increases the fatigue
substantially from 325 MPa to 875 MPa, or almost 170 %, whereas life by 40 % (machining decreases the surface roughness by around 30x
polishing (decreasing the surface roughness by more than 100x) only and polishing the surface decreases the surface roughness by ~27x).
increases the max applied stress at runout to 800 MPa, just less than 150 These effects are not as profound as those observed for SLM Ti6Al4V HIP
%. The polishing process is done by hand which can create macroscopic samples (8 vs 5 μm). The difference in surface roughness is due to the
discontinuities (unevenness) within the gauge section of the fatigue visible melt pools which were not as prevalent on the surface of
sample (this does not occur in computer-controlled machining with a Co28Cr6Mo, so it may be expected to have less impact with subsequent
lathe) and therefore alters the stress concentrations and crack initiation surface processing. In addition, the results imply the Titanium alloy has
points and is an imperfect polishing process. It is important to note that better inherent fatigue resistance in the smooth state but is more sen
the machined samples were machined down from a solid cylinder shape sitive to surface finish compared to the CoCr. The SLM Ti6Al4V HIP
whereas the polished sample was printed as a dogbone and polished samples also had a different tensile behavior than the SLM Co28Cr6Mo
directly, so there is a slight difference in the samples aside from just the samples due to the different material used.
surface finish that may be adding to lower fatigue strength in polished With the EBM Ti6Al4V samples (Fig. 8D), polishing decreased the
samples. However, compared to rougher alternatives, the properties of surface roughness by almost 160x but only increased the fatigue strength
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A. Heimbrook and K. Gall Materials Science & Engineering A 909 (2024) 146821
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A. Heimbrook and K. Gall Materials Science & Engineering A 909 (2024) 146821
Fig. 10. Correlations between A) fatigue stress at runout vs surface roughness of only Ti6Al4V samples B) fatigue stress at runout vs tensile strength C) fatigue stress
at runout vs strain at failure.
groupings for the Ti6Al4V samples Fig. 10B, with the group with the
Table 2
higher fatigue stress being the machined and polished samples for the
Sample information for fracture analysis.
wrought and SLM Ti6Al4V. On the other hand, the strain at failure (also
Sample Name Applied Stress Cycles to influenced by local stress concentrations similarly to fatigue) displays a
(MPa) Failure
positive correlation to the fatigue life (Fig. 10C) (as strain at failure
SLM Ti6Al4V HIP 350 239,592 increases so does fatigue life), except for smoother Ti6Al4V surfaces
SLM Ti6Al4V HIP + blasted 450 361,084
such as the machined and polished surfaces. This indicates that there are
SLM Ti6Al4V HIP + machined 900 793,992
SLM Ti6Al4V HIP + polished 825 66,367
other factors besides ductility influencing fatigue resistance once the
EBM Ti6Al4V 200 441,324 surface finish of a sample reaches a certain threshold (around 0.2 μm).
EBM Ti6Al4V + polished 400 356,993
wrought Ti6Al4V + machined 875 226,668 3.6. Fracture analysis
wrought Ti6Al4V + machined + 875 156,950
polished
SLM Co28Cr6Mo 400 622,406 A table representing the samples for fracture analysis as well as the
SLM Co28Cr6Mo + machined 650 451,938 failure stress and cycles to failure is displaying in Table 2. Optical mi
SLM Co28Cr6Mo + polished 550 771,522 croscope images (Fig. 11) display one crack initiation point for the
SLM Ti6Al4V HIP + 0.25 mm gyroid 225 467,370
majority of the samples in the high cycle fatigue regime with the
SLM Ti6Al4V HIP + 0.5 mm gyroid 175 925,580
SLM Ti6Al4V HIP + 0.75 mm gyroid 200 487,534 exception of the surface gyroid samples which appear to have multiple
crack initiation sites with one primary one propagating and causing
failure. SEM images (Fig. 12) display these initiation sites at the surface
and slightly different surface finishes (the effect of which is minimized or sub surface of each specimen. The EBM Ti6Al4V samples display
by polished), this suggests that the EBM process still does not have an larger defects both at or just below the surface (approximately 100 μm in
optimized enough processing temperature to offset the HIP of SLM size) which seem to be lack of fusion defects. These defects have an
samples and the deformation processing and annealing of wrought irregular and asymmetrical shape that are detrimental in fatigue. On the
samples for a better microstructure. Additionally due to the process, the fracture surface of the EBM Ti6Al4V + polished sample, a spherical pore
larger particle size in EBM creates larger defects on the surface and (indicative of a gas pore) is also present. The SLM Ti6Al4V HIP and SLM
internally. Co28Cr6Mo samples also have internal defects (regardless of mechani
cal surface post-processing) but are much smaller than the EBM defects
3.5. Fatigue trends due to the smaller particle size during processing as well as the HIP post-
processing treatment. The wrought Ti6Al4V samples appear to have the
While surface roughness exhibits an inverse correlation to the fatigue smallest crack initiation points (also having small surface area rough
strength (the rougher the surface, the lower the fatigue strength) ness measurements) and would also explain their very slightly enhanced
(Fig. 10A), at a certain point (below ~0.2 μm) the roughness effect starts performance in fatigue relative to the SLM printed titanium. These crack
to plateau in Fig. 10. The outlier in Fig. 10A is the EBM polished sample initiation points appear to be internal defects during the manufacturing
which while smooth, has other factors impeding the fatigue life such as process that are brought close to the surface during machining and
sub surface internal defects brought to the surface and a different polishing.
intrinsic microstructure. Fig. 10A highlights the inherently lower fatigue The gyroid samples had several cracks around the solid-porous
strength of the EBM material irrespective of surface finish. The best interface (where gyroid walls meets solid surface) as well as where the
performing solid sample was the SLM Ti6Al4V HIP + machined sample corner of the gyroid meets the solid surface. The cracks starting around
(~0.2 μm surface roughness with a fatigue strength of 875 MPa). The the interface could be due to the change in infill parameters during the
worst performing sample was the as-printed EBM Ti6Al4V sample (~17 printing process. It was expected for the cracks to initiate at the corner of
μm surface roughness and a fatigue strength of 175 MPa). With the gyroid and solid surfaces, since that spot has a sharper angle for
increasing the surface roughness 85x, the fatigue strength of a solid stress to concentrate. The SLM Ti6Al4V + 0.75 mm gyroid sample dis
sample decreases 5 times. This is due to the surface roughness acting as played two locations that caused failure.
micro notches and with decreasing surface roughness, the micro notches
are decreased. Therefore, the stress concentration is decreased, and 4. Conclusion
more force is required for the crack to initiate.
While each sample had varying tensile strengths, that factor did not This study investigated the effect of material (Ti6Al4V versus
correlate as strongly as surface finish, highlighting the importance of Co28Cr6Mo), manufacturing technique (EBM, SLM, Wrought), and
surface finish over tensile strength in predicting relative fatigue strength surface finish (as printed, blasted, machined, polished, added surface
or printed metals. This may be due to the tensile curves amongst the porosity) on fatigue life of solid samples. These samples were all tested
various samples being relatively similar amongst the Ti6Al4V samples in tension-tension fatigue using identical testing parameters and sample
within the same processing group. There are two distinct separate geometry. These results can help optimize surface topographies multiple
11
A. Heimbrook and K. Gall Materials Science & Engineering A 909 (2024) 146821
Fig. 11. Optical microscope images of fracture surfaces of representative A) SLM Ti6Al4V HIP variations (~5 mm in diameter) B) EBM Ti6Al4V variations (~5 mm in
diameter) C) wrought Ti6Al4V variations (~5 mm in diameter) D) SLM Co28Cr6Mo variations (~5 mm in diameter) E) SLM Ti6Al4V HIP + gyroid variations (~5.6
mm in diameter for SLM Ti6Al4V HIP + 0.25 mm gyroid, ~6 mm in diameter for SLM Ti6Al4V HIP + 0.50 mm gyroid, and ~6.6 mm in diameter for SLM Ti6Al4V
HIP + 0.75 mm gyroid).
12
A. Heimbrook and K. Gall Materials Science & Engineering A 909 (2024) 146821
Fig. 12. SEM images of fracture surfaces of representative A) SLM Ti6Al4V HIP variations B) EBM Ti6Al4V variations C) wrought Ti6Al4V variations D) SLM
Co28Cr6Mo variations E) SLM Ti6Al4V HIP + gyroid variations.
sensitive to the presence of surface roughness, seeing a larger drop in draft, Visualization, Validation, Investigation, Formal analysis, Data
fatigue strength with the addition of a rough surface. curation. Ken Gall: Writing – review & editing, Supervision, Resources,
7. Mechanical post processing improved fatigue strength across all Project administration, Funding acquisition, Conceptualization.
sample groups, but after a critical surface roughness of about 0.2 μm,
further decreasing the surface roughness is relatively ineffective in Declaration of competing interest
increasing fatigue strength.
8. Adding 0.25 mm of porous gyroid to the surface of a SLM Ti6Al4V The authors declare the following financial interests/personal re
HIP sample yields a lower fatigue strength than rough as-printed SLM lationships which may be considered as potential competing interests:
surfaces, but higher fatigue strength than the solid samples with the Ken Gall reports a relationship with restor3d that includes: board
roughest as-printed surface (EBM Ti6Al4V). Increasing gyroid membership, employment, and equity or stocks. If there are other au
thickness had a limited additional impact on fatigue strength. thors, they declare that they have no known competing financial in
9. In HCF, samples failed from surface or sub surface defects with EBM terests or personal relationships that could have appeared to influence
samples displaying the largest surface and internal defects, including the work reported in this paper.
gas pores.
Data availability
CRediT authorship contribution statement
Data will be made available on request.
Amanda Heimbrook: Writing – review & editing, Writing – original
13
A. Heimbrook and K. Gall Materials Science & Engineering A 909 (2024) 146821
Acknowledgement of funding sources [22] A.B. Novaes Jr., S.L. S.d. Souza, R.R. M.d. Barros, K.K.Y. Pereira, G. Iezzi,
A. Piattelli, Influence of implant surfaces on osseointegration, Braz. Dent. J. 21
(2010).
This work was performed in part at the Duke University Shared [23] I.S. Grech, J.H. Sullivan, R.J. Lancaster, J. Plummer, N.P. Lavery, The optimisation
Materials Instrumentation Facility (SMIF), a member of the North Car of hot isostatic pressing treatments for enhanced mechanical and corrosion
olina Research Triangle Nanotechnology Network (RTNN), which is performance of stainless steel 316L produced by laser powder bed fusion, Addit.
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