Additive Manufacturing 29 (2019) 100779

Contents lists available at ScienceDirect

Additive Manufacturing
journal homepage: www.elsevier.com/locate/addma

Review

Overview: Additive Manufacturing Enabled Accelerated Design of Ni-based T

Alloys for Improved Fatigue Life
⁎
S. Shaoa, , M.M. Khonsaria, S. Guoa, W.J. Menga, N. Lib
a
Department of Mechanical and Industrial Engineering, Louisiana State University, Baton Rouge, LA, 70803, United States
b
Center for Integrated Nanotechnologies, Los Alamos National Laboratory, Los Alamos, NM, 87545, United States

A R T I C LE I N FO A B S T R A C T

Keywords: An in-depth overview on an emerging area of the additive-manufacturing-enabled, accelerated design of Ni-
High-frequency fatigue testing based alloys for improved high-cycle and very-high-cycle fatigue life is presented. Existing literature on the
Ni-based alloys subject is critically reviewed, and key knowledge gaps are identified. An efficient life-cycle approach, integrating
High-cycle/very-high-cycle fatigue the model-make-measure-verify strategy in the design of these alloys is introduced and discussed.
Additive manufacturing enabled technologies
Persistent slip band

1. Introduction improvement in fatigue properties of AM alloy parts therefore not only

Ni-based alloys are a class of precipitation- and solid solution-
hardened alloys that possess exceptional high-temperature strength as
well as creep and corrosion resistance [1]. They find use in extreme
environment applications such as gas turbine blades/discs, high-tem-
perature heat exchangers in nuclear reactors, and high-temperature
components of petrochemical plants. Ni-based alloys, however, suffer
from poor machinability. To minimize the need for conventional sub-
tractive machining, manufacturing components made of those alloys
typically involve wrought, cast and powder metallurgy [1]. However,
these techniques typically cannot produce parts with complex geome-
tries or shapes. Additive manufacturing (AM) offers a cost-effective
remedy. It enables the near net-shaping of Ni-based alloy parts by a
bottom-up, layer-by-layer fabrication strategy [2].
The fatigue performance of present additively manufactured (AM)
metal parts are inferior to that of their wrought counter parts, causing
growing concerns toward the applicability of AM technology to key
engineering components [3–11]. Indeed, as fabricated AM parts often
contain many non-equilibrium phases and defects, from atomic level
point defects to non-equilibrium phases, pores, and flaws [12,13].
These features can raise the local stress level to the point where plastic
strains occur. During cyclic loading, the number and intensity of local
slip bands increase and cause microstructural damages that shorten
service life [14]. Further complexities arise from the fact that the alloys
currently utilized in AM were generally not optimized for laser-based
AM processes [15,16]. These factors compromise the mechanical in-
tegrity and challenge quality certification of AM parts. The
relies on the optimization of AM processing parameters to minimize the
AM defects, but also on the redesign of alloys’ composition/micro-
structures to enhance fatigue resistance. Moreover, efficient adoption of
AM parts also requires the development of rapid certification meth-
odologies based on accelerated fatigue testing.
Significant research efforts documented in the literature align, to
various extents, with two research directions: alloy development
[11,17–20] and rapid certification [7,21–32]. Successful implementation
of these approaches offers an immense potential for introducing rapidly
qualified materials with superior properties for use in AM components
that can be readily deployed in the field. A review of the literature
reveals, however, that considerably less research has been attempted to
address properties and certification methodologies of Ni alloys. This is
surprising since these alloys are more pertinent to engineering appli-
cations [1,2,33]. For instance, concerning alloy development in gen-
eral, much research has been conducted to tailor alloys’ composition,
microstructure, and architecture targeting better melt pool character-
istics and, in turn, mechanical performances [11,17–20]. However, the
focus on mechanical properties has been mostly on monotonic ele-
ments, i.e. rigidity, tensile strength, ductility and hardness, etc. Strate-
gies for development of AM materials with cyclic fatigue resistance—-
which has significant engineering-relevance—is less studied.
Research concerning rapid certification methods has been largely
devoted to online melt pool monitoring [7,21,25], defect character-
ization [22,23,26–32], numerical modeling of AM processes [21,24],
and in-situ process control [25]. These approaches are particularly
important to improve parts’ quality at critical locations for accelerated

⁎
Corresponding author.
E-mail address: sshao@lsu.edu (S. Shao).

https://doi.org/10.1016/j.addma.2019.100779
Received 18 April 2019; Received in revised form 16 June 2019; Accepted 2 July 2019
Available online 21 July 2019
2214-8604/ © 2019 Elsevier B.V. All rights reserved.
S. Shao, et al.
Fig. 1. A flow chart summarizing prevailing literature in AM with references
discussed in this overview added (in blue).
certification. However, actual fatigue life evaluations on AM materials
still mostly rely on conventional fatigue testing [2,5,9,27,30,34–46]
which can be expensive, time-consuming, and limited to low number of
cycle (typically < 107). Accelerated life-evaluation based on high-fre-
quency tests has so far received much less attention [47]. Relevant
research activities concerning Ni-based alloys is even less frequent [48].
To add to the utility of this overview article, the prevailing AM litera-
ture, as briefly reviewed above, are given in Fig. 1 in the form of a flow
chart with references added.
A unique research direction, i.e. AM-enabled, accelerated design of
Ni-based alloys for enhanced fatigue performance in the high-cycle-
fatigue (HCF) and very-high-cycle-fatigue (VHCF) regimes through fine
controls in the alloy composition and microstructure, appears to be
presently underexplored by the AM research community, despite its
engineering relevance. VHCF, with typical failure cycles in the range of
Nf = 109, becomes increasing relevant for modern engineering appli-
cations, such as high speed rails. The intertwined nature of fine-tuning
calls for multifaceted and iterative research involving: development of
defect and microstructure sensitive fatigue models, rapid manu-
facturing of alloy samples with variable composition and micro-
structure, rapid evaluation of life and damage accumulation in HCF and
VHCF, and, importantly, model validation (see Fig. 2). Historically,
Fig. 2. A potential framework for accelerated alloy development enabled by custom powder synthesis, additive manufacturing and variable frequency fatigue testing.
2
Additive Manufacturing 29 (2019) 100779
systematic integration of these research tasks appeared daunting, for
the lack of capabilities in numerical materials modeling, accelerated
fabrication, and accelerated fatigue testing of specimens [49]. With
recent developments in powder synthesis [50–57], custom metal AM
[58–62], as well as ultrasonic fatigue testing techniques [49,63–67],
opportunities for addressing these needs are ripening in terms of the
technologies and the scientific knowledge. At present, the AM research
community appears to be in a unique position to undertake such a task.
In this overview article, we primarily focus on the prior literature
pertinent to this unique research direction— the AM-enabled, ac-
celerated Ni-superalloy optimization for HCF life. The Ni-based alloys
discussed in this article are limited to the γ-γ’ alloys, due to their well-
studied microstructure and good tunability with a wide space of al-
loying elements—raising the hope that the material properties can be
adjusted relatively independently.
This article is organized as follows. In Section 2, common fatigue
damage mechanisms of metals, especially FCC and FCC-like metals
operating in the HCF regime are briefly discussed. In Section 3, a dis-
cussion on the effect of frequency on fatigue damage evolution is pre-
sented. Section 4 reviews pertinent efforts in the enhancement of fa-
tigue resistance in Ni-based alloys via microstructural/compositional
tuning. In Section 5, the various fatigue models are briefly discussed.
Knowledge gaps in the current understanding, which may hinder the
effective development of Ni-alloys for AM, is summarized in Section 6.
Section 7 is devoted to potential opportunities in optimizing HCF per-
formance of Ni-alloys. Of particular interest is the assessment of the
entire lifecycle of such alloys via computation-guided alloy design,
custom alloy powder synthesis, laser AM, comprehensive materials
characterization, accelerated in-situ/ex-situ fatigue testing, and model
validation. These are addressed in Section 8. An outlook on future’s
research directions in AM has been provided in Section 9, followed by
concluding remarks in Section 10.
2. Fatigue damage mechanisms in FCC/FCC-like metals
Fatigue cracks in metals are initiated by slip. In HCF/VHCF regimes,
the initiation stage of fatigue cracks is especially important as it can
account for up to 90%, or higher, of the total fatigue life [68–70]. In
this regime, localized plastic deformation occurs due to the presence of
materials’ imperfections and elastic incompatibility across grain
boundaries (GBs), even though the macroscopic mechanical response
appears to be elastic [68,71–73]. The presence of defects such as pores
and the associated stress concentrations causes localized plastic de-
formations and subsequent development of slip activities (slip bands)
even at very low applied cyclic strain ranges [14]. Therefore, as com-
pared to wrought materials, AM materials usually exhibit a significantly
S. Shao, et al.
reduced fatigue life due to accelerated fatigue crack initiation (FCI).
Mechanistically, the FCI under the regimes of HCF/VHCF and low-
cycle-fatigue (LCF) are indistinguishable. However, as the magnitude of
the localized plastic strain near the GBs and the flaws are smaller
compared to the global plastic strain under the LCF regime, the FCI
under HCF/VHCF takes substantially more cycles to accomplish (hun-
dreds of thousands of cycles at Nf = 106 cycles vs around a few thou-
sand cycles at Nf = 103˜104 cycles). In addition, while multiple in-
itiations of fatigue cracks are common in LCF, initiation of single crack
is dominant under HCF and VHCF. There also tend to be a shift of in-
itiation sites from exterior to interior under VHCF [63].
Abundant literature on the evolution of materials’ microstructure
during cyclic plasticity leading to fatigue crack initiation is available. A
comprehensive review on the formation mechanism of dislocation ar-
rangements in FCC single crystals under cyclic loading has been pub-
lished before [74]. Typical local cyclic response of a material involves
an initial, rapid hardening phase followed by a saturated phase with a
much more gradual change in the cyclic stress-strain response that ty-
pically constitutes a cyclic softening stage [75–77]. During the initial
hardening phase, the dislocations rapidly multiply via Frank-Read
sources, leading to an increased dislocation density. Continued increase
in the dislocation density within the grains leads to the formation of
veins (such as ones shown in Fig. 3a [78] and as depicted in Fig. 3b)
with interconnecting screw dislocations.
Continued accumulation of dislocations gives rise to cyclic softening
due to the widening of the channels associated with the formation of
persistent slip bands (PSBs) (Fig. 3a and c) [79–82]. From this stage, the
overall plastic deformation of a specimen is dominated by the localized
shear deformation in the PSBs (Fig. 3c) [84–87], which is accom-
modated by the to-and-fro motions of pure screw dislocations between
the sub-grain dislocation dipolar walls (Fig. 3c) [81,85,88–90]. The
irreversibility of the cyclic plastic deformation is due to the events in-
terrupting dislocations’ back-and-forth motion, such as cross-slip and
annihilation [84,91–93]. These events are thermally-activated, rate-
dependent occurrences whose activation energy is also material-de-
pendent (such as stacking fault energy (SFE) or antiphase boundary
energy (APBE) [1,94–98]). For polycrystalline materials—since high-
angle grain boundaries (GB) are typically impenetrable to PSBs—the
fatigue strength is inversely related to its average grain size [99–103].
Fig. 3. (a) Typical microstructure of single crystal Cu under fatigue loading
[78]. (b) Schematic illustration of vein structure and (c) Formation of PSB
[79–83].
3
Additive Manufacturing 29 (2019) 100779
In Ni alloys, the γ’ precipitates has an ordered L12 structure which
strongly restricts the motion of dislocations [104–106], resulting in
PSBs with substantially different structures from pure FCC metals.
Eventually, continued operation of PSBs accumulates sufficient amount
of damage, which lead to fatigue crack initiation (FCI) [73,107–109]
either at GBs (due to inter-granular deformation incompatibility) or
surfaces (due to intrusion/extrusion mechanism). The mechanism of
fatigue crack initiation from PSBs is identical in both γ-γ’ alloys and in
pure FCC metals. Within the life cycle of PSBs, the dislocation density
tends to increase and eventually saturate to a critical value at which FCI
occurs [75–77]. This observation agrees with the semi-empirical model
developed by Tanaka and Mura, which states that fatigue cracks initiate
when a critical dislocation-interaction energy is reached due to the
systematic accumulation of dislocation dipoles in a PSB [110,111].
Thus, the retardation of the FCI through active intervention in mi-
crostructure and composition may offer an avenue for extending the
fatigue life of AM metals. However, quantitative knowledge on how the
microstructure and composition influences the operation of PSBs and
the subsequent initiation of fatigue cracks is presently lacking.
3. Effect of loading frequency
Rate-dependent, “interruptive” events, such as cross-slip and anni-
hilation alter the dislocations’ paths and increase the irreversibility of
the cyclic plasticity [90,112]. For FCC (or FCC-like) materials, an im-
portant factor affecting the rate of cross-slip and annihilation is the
stacking fault energy (SFE) or anti-phase boundary energy (APBE). As
perfect dislocations always dissociate into partial dislocations in FCC
crystals, i.e. a pure screw dislocation exists as two mixed Shockley
partials enclosing a stacking fault. (Similarly, pairs of super partial
dislocations are always separated by antiphase boundaries in L12
structures [1].) For cross-slip (or annihilation) of this screw dislocation
to occur, two partial dislocations need to first recombine under thermal
activation (Escaig’s model [113,114]). The probability of recombina-
tion depends on the equilibrium spacing between the two partials,
which, in turn, is dictated by the SFE/APBE. Therefore, the rate of the
interruptive events is ultimately governed by SFE/APBE [115,116]:
τ* − τ ⎞
JInt. = A0 ν0exp ⎛−
⎜ V and V= αD02 b
⎟
⎝ kT ⎠ (1)
where A0 is the total number of available screw segments, ν0 is the
attempt frequency factor, τ* is the critical stress for cross-slip, τ is the
resolved shear stress (RSS) in a given slip plane, V is the activation
volume, α is a material dependent constant, k is the Boltzmann’s con-
stant, and D0 is the spacing between partial dislocations, which is a
function of the SFE (or APBE), i.e. D0 = μb2 /4πγSFE . In the expression for
D0, μ is the shear modulus of the material, b is the magnitude of the
Burgers vectors of Shockley partials.
Due to the rate-dependent nature of cross-slip and annihilation, low-
(high-) frequency cyclic loadings that allow more (less) time for them to
occur are associated with greater (less) damage and irreversibility. At
higher frequencies, the rate-dependent events do not have sufficient
time to occur. As a result, “plastic deformation” at these frequencies is
more “reversible” [117,118]. In other words, the to-and-fro motions of
screw dislocations in the PSBs are less likely to be interrupted, so that
much less debris due to dislocations’ activities are left behind in the
form of immobile dislocations [119]. Therefore, the damage induced by
the high-frequency testing is expected to be considerably less than that
of the conventional low-frequency testing, even though the hysteresis
energy might be the same. The concept of slip reversibility also applies
for fatigue crack propagation studies. Therefore, results from ac-
celerated fatigue testing at frequencies of several to tens of kHz may not
correlate well with true service conditions at frequencies of only tens of
Hz. Conversely, fatigue testing conducted under low frequencies, may
not reflect the life of parts under high-frequency service conditions
S. Shao, et al.
Fig. 4. (a) Dark-field TEM micrograph showing the γ’ precipitation structure of René 77 alloy [1]. (b) Fatigue crack propagation response of small γ’ fraction alloys
[136,137].
[120–125]. This is especially true for Ni-based superalloys due to their
thermally activated nature in the plasticity leading to their strong fre-
quency and temperature dependent fatigue behavior [123–126]. Eq. (1)
also indicates that the effect of test frequency on the deformation be-
havior can be strongly composition-dependent (via SFE/APBE)
[120–122]. While the frequency effects on fatigue life of wrought alloys
have been extensively investigated [120–125,127,128], such effects on
AM alloys, where the composition and microstructure can be vastly
different, have seldomly been investigated [47,129]. Therefore, further
research efforts should be directed to the assessment of frequency ef-
fects on the AM Ni-superalloys, as a function of microstructure, to
provide robust correlation between accelerated fatigue tests and the
true service life of these alloys.
4. Effect of composition and microstructure
The Ni-alloys, while complex compositionally, have unique micro-
structures (Fig. 4a) [1,130,131]. They typically consist of a solid solu-
tion strengthened Ni γ matrix, cuboid-shaped Ni3Al based γ’ pre-
cipitates with a L12 structure, and various carbides. For polycrystalline
alloys, carbides typically form at GBs and provide strong resistance to
GB sliding, improving the alloys’ creep resistance [132]. For single
crystal alloys, addition of carbon can improve the alloys casting char-
acteristics [133]. However, carbides are brittle and very effective in-
itiation sites for fatigue cracks. Therefore, they are detrimental to the
fatigue resistance of Ni-superalloys [134]. Other alloying additives,
such as Ti and Mo, can be added to increase the SFE and APBE of the γ
matrix and γ’ precipitates. Other elements can also be added to adjust
the γ/γ’ lattice mismatch (e.g., Mo) and to provide solid solution
strengthening of the matrix (e.g. W, Ta, Mo, and Cr). The size of the
precipitates as well as the grain size can be controlled by employing
various heat-treating schedules. Generally, the size, and morphology, of
the γ’ precipitate is influenced by the cooling rate below the solvus
temperature. The size of the precipitate is also affected by aging time.
The γ’ volume fraction is dictated by the composition. The grain size
can be controlled by means of forging, with subsequent recrystallization
procedure at temperatures above solvus.
The notion of achieving enhanced fatigue resistance via composi-
tional and microstructural adjustments dates back to almost three
decades ago [135–137]. These works have shown, importantly, that the
fatigue crack propagation (FCP) rate is especially low for alloys with
low APBE, low precipitate/matrix lattice mismatch and low volume
fraction of precipitates (alloy 1 in Fig. 4b) [136,137]. However, due to
the limitations in both computational and experimental resources at
4
Additive Manufacturing 29 (2019) 100779
that time, establishing the precise correlation between the composi-
tion/structure and fatigue performance of Ni-based alloys were asso-
ciated with high cost in equipment, materials and time. Thus, generally,
the reported findings were largely qualitative in nature. In addition,
although these findings have important implications on the FCP of Ni-
based alloys, knowledge regarding the microscopic FCI behavior—-
which operates under a different mechanism—is still largely lacking.
Recently, attempts have been made toward tailoring the fatigue
performances of Ni-based alloys via optimizing forging processes [92].
This approach was supported by a physics-based framework on the
prediction of crack initiation based on the energy evolution in PSBs
[93]. Such a framework is quite promising as it accounts for the effects
of many of the underlying physics responsible for the operation of PSBs
[92,93] such as dislocation pile-up, work-hardening, nucleation of
dislocations from GBs, precipitation, as well as the interaction between
PSBs with GBs, etc. However, the description of many of these physical
mechanisms is still largely empirical in nature. In addition, a key ele-
ment— the contribution of dislocations’ self-energy—is yet to be ac-
counted for.
Research on investigating supperalloys’ compositional and micro-
structural effects has mostly focused on conventionally manufactured,
such as casted or forged, alloys. The typical microstructure of as-built
AM Ni superalloys, due to the associated high cooling and solidification
rates, has vastly different, but highly non-equilibrium, microstructure,
featuring elongated grains containing micron-width dendrites (for γ/γ’/
γ” alloys such as Inconel 718 [138–140]) or nano-sized precipitates (for
γ/γ’ alloys such as Inconel 939 [141]). Research efforts targeting fa-
tigue properties of Ni superalloys [2,5,9,10,142] have been con-
siderably less than other AM alloys, e.g. Ti-6Al-4 V. Research addressing
the effect of as-built microstructure of AM Ni superalloys on their fa-
tigue performance has been scarce and further investigations are
needed.
To sum, precise composition/structure – property correlation for Ni
superalloys, especially for AM Ni superalloys, is still incomplete.
Consequently, efficient alloy design still remains challenging.
5. Fatigue modeling in the HCF/VHCF regimes
Classical experiment-based macroscopic fatigue models [143], such
as the cycle counting methods [144,145] and energy-based methods
[146–148], are largely empirical in nature and rely on the construction
of fatigue data based on extensive fatigue testing. Thus, the predictions
made by many of the available models are limited on the specific ma-
terials and test conditions considered. The generalization of those
S. Shao, et al. Additive Manufacturing 29 (2019) 100779

models to a broader range of materials and testing conditions are ty-
pically ineffective, as it would require considerable re-testing. In ad-
dition, an important phenomenon in the cyclic deformation—reversi-
bility (a quite complex parameter that depends on both material and
loading condition [84,117,118,149–151])—is either ignored or treated
empirically. As a result, a great majority of the existing models cannot
reliably account for variations in materials’ susceptibility to damage or
accurately predict the effect of the loading frequency. For instance,
nano-twinned metals have recently been shown to exhibit extreme
cyclic stability and damage resistance, even under LCF conditions
[151]. Moreover, their cyclic reversibility is substantially greater at
higher loading frequencies [84]. Clearly, physics-based fatigue models
that can be readily applied to a larger materials space and predict these
features are needed.
It has been recently demonstrated that the application of irrever-
sible thermodynamics can further elucidate the process of metal fatigue
[152–157]. For instance, the nucleation of fatigue cracks can be treated
as a thermally activated process, and this be predicted using classical
nucleation theory [156,157]. In addition, as cyclic loading irreversibly
degrades the system until the final failure, the second law of thermo-
dynamics may be uniquely suitable for characterizing the evolution of
the associated fatigue damage. Indeed, it has been shown that a strong
correlation exists between the fatigue degradation and entropy gen-
eration and that a critical cumulative entropy is reached at the point of
fracture. This parameter—referred to as fracture fatigue entropy (FFE)
[158]—is a material constant that is independent of sample geometry,
loading conditions and frequency. The applicability of this principle to
a broader range of materials, including composite laminates where the
respective FFEs are constant in the fiber and the matrix, has already
been demonstrated [159].
HCF/VHCF deformation is mostly elastic as the stress amplitude is
well below the yield strength of the material. In this case, the reversible
portion of the inelastic deformation, referred to as internal friction by
some, accounts for a substantial portion of the hysteresis energy. The
irreversible portion of the hysteresis energy is damaging and is re-
sponsible for the FCI [160]. As the hysteresis energy in the HCF/VHCF
is minuscule, discerning its damaging and non-damaging, i.e. the in-
ternal friction, portions by the conventional energy-based fatigue
models is challenging. Recently, a novel methodology that uses energy
dissipation as a fatigue damage indicator was developed to account for
the effect of internal friction [161]. Following this methodology, the
initial slope of the surface temperature rise as a function of time (Rθ)
can be decomposed into contributions of the internal friction (Rθf ) and
the irreversible portion (Rθp ) [162–164], i.e.,
DD to fatigue damage could only cover tens of cycles. While this may be
sufficient for the investigation of initial stages of HCF— e.g. initial
cyclic hardening behavior [170–172], or behavior of cracks under very
low-cycle fatigue regions, e.g. crack initiation crack propagation
[173–178]— the analysis of the evolution of cyclic mechanical response
in the HCF/VHCF regimes are presently inaccessible.
6. Present knowledge gaps
Efficient optimization of Ni-based (γ-γ’) alloys not only requires the
technology of accelerated fabrication (such as AM) and testing (such as
high-frequency fatigue testing), it also requires accurate fatigue damage
modeling that can properly account for the effects of loading frequency
and microstructure/composition on fatigue damage evolution.
However, as discussed in the foregoing sections, significant knowledge
gaps exist in the fundamental understanding of these mechanisms. The
lack of this understanding is even more pronounced in AM Ni super-
alloys. Paucity of information mainly concerns with the rate-dependent
operation of PSBs as a function of materials’ microstructure and com-
position, not only in conventionally manufactured alloys but also—-
more importantly—in AM alloys. These gaps can be summarized as
follows:
- How do fine adjustments in alloy composition, phase composition,
and microstructure on laser AM Ni-based alloy parts affect the cyclic
behavior of dislocation arrays?
- How does the test frequency affect the cyclic behavior of dislocation
arrays for laser AM Ni-based alloy parts, under the influence of the
aforementioned materials parameters?
7. Optimizing HCF/VHCF performance of Ni-alloys – a few
opportunities
In a recent dislocation dynamics (DD) modeling-based research
[84], it was shown that the cyclic deformation reversibility is directly
correlated with fatigue damage accumulation. In addition, the cyclic
deformation reversibility in the PSBs was found to depend strongly on
both the material and the loading frequency (Fig. 5). At a given loading
frequency, the deformation reversibility of a material is dependent on
its SFE. A lower (higher) SFE leads to lower (higher) rate of cross-slip/
annihilation, which then correspond to higher (lower) deformation

Rθ = Rθf + Rθp (2)

Accordingly, the FFE can be evaluated as

Nf Rθp ρcp
FFE =
fTs (3)

where Nf is the number of cycles to fatigue failure, Ts is the steady state

temperature, f is the loading frequency, ρ is the mass density of the
sample, cp is the isobaric heat capacity.
In HCF/VHCF regimes, the evolution of dislocation structures gov-
erns the cyclic stress-strain response as well as the initiation of fatigue
cracks. Therefore, effective meso- and continuum- scale modeling
[165,166] of the fatigue behavior of materials under these regimes
would inevitably require an a priori knowledge regarding the disloca-
tion evolution from the lower length scale models, e.g., via discrete
dislocation dynamics (DD) models. However, the computational cost of
conventional DD calculations increases with the buildup of the dis-
location density (number of integration points on dislocation lines),
which rises significantly due to the dislocation multiplication me-
chanisms under cyclic loading. Given that the time scale of DD is se- Fig. 5. Effect of cross-slip and loading frequency on the dislocation density in
verely limited [167–169], presently the conventional applications of PSBs, obtained from a dislocation dynamics modeling-based study [84].

5
S. Shao, et al.
reversibility. This is apparent when comparing the red (#3) and the
magenta (#5) curves in Fig. 5, which represents the cyclic evolution of
excess dislocation densities in the PSBs for two materials with high
(magenta, #5) and extremely low (red, #3) SFE. Note that the case #5
accumulates damage (measured by dislocation density) at a sig-
nificantly higher rate. The improvement of both HCF and LCF fatigue
performances due to the reduction of SFE has been clearly demon-
strated by nanostructured, Cu-based binary alloys [179].
For a given material, increased loading frequencies tend to induce
higher cyclic reversibility as well as lower cyclic damage and, hence,
longer fatigue life. This is also evident in Fig. 5, which shows that with
the same rate of cross-slip, the lower frequency case (#5, magenta
curve) results in more damage per-cycle compared to the case of high
frequency (#2, green curve). The higher fraction of reversible cyclic
deformation was attributed to two aspects: (1) Due to the higher im-
posed strain rate, the dislocation structure does not have sufficient time
to fully relax, via dislocation gliding motion. As a result, much of the
total deformation is accommodated by elastic/anelastic deformations
leading to a much lower hysteresis energy; (2) Due to the significantly
shortened time scale imposed by the higher loading frequency, rate-
dependent events, such as cross-slip/annihilation, do not have sufficient
time to impact the to-and-fro motion of the runner dislocations, leading
to a higher cyclic reversibility. This work also demonstrated the im-
portance and necessity of incorporating cyclic reversibility into fatigue
models.
A unique opportunity presents itself for accurately predicting the
HCF and VHCF life of alloys by incorporating the notion of cyclic de-
formation reversibility. It can be postulated that any situation—mi-
croscopic features and/or loading conditions—that promotes more re-
versible cyclic deformation would lead to a longer HCF/VHCF life. For
instance, lower SFE and APBE (for the case of easy-shear precipitates) is
expected to improve the HCF/VHCF resistance of Ni-based alloys.
Similarly, reducing the mean free paths of dislocations without indu-
cing dislocation multiplication could also increase the cyclic deforma-
tion reversibility. For instance, grain refinement is a good candidate,
since high fractions of GBs can reduce the dislocation density by re-
ducing the number of participating dislocations in pile-ups [68,99].
Indeed, available data in the literature reveal that materials’ HCF
strength is inversely proportional to its grain size [180–182]. This
finding agrees well with the model proposed by Tanaka and Mura
[101,111] who showed that a Hall-Petch type relation exists between
HCF fatigue strength and grain size. Also, a well-aligned, hard-to-shear
γ’ precipitates (with high APBE and/or high γ’/ γ lattice mismatch)
[1,137] may also serve such a purpose. These postulations are exciting
in that, if proven to be correct, the resulting Ni-based alloys would have
both high yield strength and HCF/VHCF strength—properties desirable
for AM materials. This is in contrast to the conclusions drawn in the FCP
studies [135–137] where microstructures with larger grains, lower
volume fractures of precipitates, lower lattice mismatch are thought to
yield higher fatigue resistance.
Moreover, since cross-slip and annihilation are the main events re-
sponsible for cyclic irreversibility [91,92,101–103,183–185], the
amount of damage accumulated per cycle () is expected to be pro-
portional to the number of the interruptive events occurring per cycle,
i.e.  ∝ JInt./ f , where f is the cyclic frequency. Therefore, the frequency
effect is also expected to be dependent on the SFE and APBE, among the
characteristic microscopic dimensions discussed above. This postulate,
if proven to be true, has profound engineering implications for AM Ni-
based alloys, since it suggests that a simple mathematical relation may
exist to bridge the frequency discrepancies between the true service
conditions and lab testing conditions.
8. A model-make-measure-verify based life-cycle approach
Efficient optimization of the HCF/VHCF performance of AM Ni-
based alloys may be achieved by synergistic integration of the complete
6
Additive Manufacturing 29 (2019) 100779
Fig. 6. Closed M3V loop materials design approach featuring the entire life
cycle of an AM part, including alloy design, powder production, 3D printing,
mechanical/fatigue testing, and multiscale computational fatigue damage
model development.
life cycle of these alloys, namely a model-make-measure-verification
strategy (Fig. 6).
In the model stage, a predictive, physics-based fatigue model, cog-
nizant of the alloys’ materials properties, including SFE, APBE, pre-
cipitate/matrix lattice mismatch, spacing and volume fraction of pre-
cipitates capable of tracking the evolution of fatigue damage in the
HCF/VHCF regimes is highly desirable. As the manifestation of various
materials properties to materials overall fatigue response is multiscale
in nature, such a fatigue model may involve successive information-
passing between multiple length scales. As the SFE and APBE may di-
rectly influence the rate of cross-slip, atomic scale calculations are ne-
cessary. Limited by the available semi-empirical interatomic potentials,
most of which are for binary or ternary systems [186], molecular dy-
namics/statics calculations on the SFE and APBE is currently not fea-
sible for these alloys, which typically contain ˜10 elements. Limited by
the size of the computational cells, direct density functional theory
(DFT) cannot fully address the long range dis-ordering occurring within
the alloys [187,188]. More advanced methods have to be applied for
this purpose. For APBE of the γ’ phase, the most promising method is
the density functional theory (DFT) based cluster expansion (CE)
method combined with Monte Carlo (MC) sampling. CE [189] para-
metrizes the configuration-dependent energy of an alloy, by first ab-
stracting the alloy’s atomic structure into a lattice model then expres-
sing the energy into a polynomial form of the occupation states. After
CE, MC sampling can be performed on thousands of lattice structures,
each containing thousands of atoms, to account for the effect of che-
mical disordering. For SFE of γ phase, direct CE/MC is not applicable
since the stacking faults does not obey the symmetry of the FCC parent
lattice. Therefore, a hybrid method combining CE/MC with one-di-
mensional Ising (1DI) model [190] is needed.
It has been shown by various studies that, under cyclic loading,
dislocation density in metals monotonically increases [75–77,191,192].
It was further shown by Pangborn et al. [191] that fracture occurs when
a critical excess dislocation density is exceeded. It was also shown by
the same group [191] that since the dislocation density rises steadily up
to this critical value under cyclic loading, the fatigue damage of a
material at any stage of life could be determined. Dislocation density
S. Shao, et al. Additive Manufacturing 29 (2019) 100779

can therefore be used as a fatigue damage parameter. Models capable of

tracking the evolution of dislocation densities in the PSB structures,
such as DD or continuum scale DD [193–195], therefore may accurately
track the evolution of fatigue damage of Ni-alloys. However, the con-
tinuum level DD models require the evolution laws of dislocation
density a priori, which are necessarily obtained from DD models. In HCF
and VHCF regimes, formation of PSBs occurs at a very early stage of
cyclic loading [63]. While full simulations may be computationally
prohibitive, opportunities to develop coarse-grained (CG) DD are
available if the treatment of “runner” dislocations and wall dislocations
is decoupled. In other words, if runner dislocations are simulated by
conventional DD while dislocation walls are treated as specialized
planes capable of tracking dislocation density.
In the make stage, informed by physics-based fatigue models,
custom alloys can therefore be rapidly fabricated via various AM plat-
forms [196] in combination with custom powder synthesis. Various
materials parameters, such as SFE/APBE, lattice mismatch, volume
fraction of γ’ and grain size can be adjusted by fine-tuning the relative
concentration of the constituents of the AM alloy with the application of
subsequent heat treatments. By actively adjusting the processing para-
meters, orientation and the cooling rate, the microstructure of the AM
parts can also be fine-tuned [32,197]. It has been shown [32] that the
alteration in the build parameters (such as laser power, layer thickness,
scan velocity and laser focal offset) and post-build treatments can
produce an extremely fine grain size (˜ hundreds of nanometers). Si-
milar effects were achieved via the in-situ printed heat sink technique
during selective electron beam melting [197], where sacrificial heat
sinks were attached to the printed parts by design.
SFE and APBE can be adjusted by varying weight percentages of
some key elements. Mo and Cr may be used as the main additive to tune
the SFE in the γ matrix, as well as to provide solid solution strength-
ening. The strong effect of Mo on the SFE of the Ni-Mo system is well
documented [198]. APBE of the γ’ precipitates may be adjusted by
tuning the ratio of Ti/Al, as it has been shown that the APBE directly
correlates with this ratio [199]. Using this approach, the SFE of γ and
the APBE of γ’ can be adjusted relatively independently.
8.1. Lattice mismatch
Adjustments of the SFE and APBE require introducing solid solu-
tions, which would inevitably alter the lattice constants of the phases.
Within the solubility limits of various additives in Ni, the γ/γ’ lattice
mismatch is very small [137,200]. Although the change in the absolute
mismatch due to the compositional adjustments is small, studies [137]
have shown that a slight change in the APBE (by a factor of 1.3) has
induced a 20-fold change in the γ/γ’ mismatch. While keeping the APBE
relatively constant (small changes in the Al/Ti ratio), the lattice con-
stant of γ’ can be independently adjusted by controlling the level of Ti.
In addition, Mo can also be varied slightly for this purpose. As a result,
the mismatch can be adjusted relatively independently.
8.2. Volume fraction, size, and morphology of γ’ precipitates
This volume fraction is dependent on the available Al and Ti, as the
γ’ phase mostly maintains a well-defined stoichiometry. Therefore, a
moderate change in the volume fraction of precipitates can be achieved
by tuning the Al/Ti contents. Note that this may lead to a change in the
lattice constant of the γ’ phase. The size and morphology of the pre-
cipitates can be adjusted by cooling rate below solvus temperature and
subsequent aging time. High cooling rate typically lead to spherical
morphology while lower cooling rates lead to cuboidal morphology
[201]. The size of the precipitates can be controlled with varying aging
times.
In the measure stage, the materials features of the samples resulting
from the “make” stage can be characterized through a combination of
materials characterization techniques including X-ray diffraction
Fig. 7. (top) Schematic diagram of the vibratory fatigue tester. (bottom left)
Snapshot of sample during test. (bottom right) Operating resonant frequency as
a function of sample length (material shown is Cu) [202,203].
(XRD), scanning and transmission electron microscopy (SEM/TEM),
and electron backscatter diffraction (EBSD). In this state, fatigue per-
formances of Ni-alloys with varying materials are also examined at
varying testing frequencies. Various types of conventional fatigue
testing platforms, such as bending, torsion, and push-pull, can be used
to study the fatigue damage accumulation of Ni-alloys using standard
mechanical testers with frequencies f < 20 Hz. Effect of loading fre-
quency can be evaluated by subjecting the same samples to high fre-
quency tests.
To assess the effect of testing frequency on the fatigue behavior of
AM Ni-alloys, various state-of-the-art, piezoelectric based platforms can
be used [49]. These testers can work in tension-compression, tension-
tension and bending, and reach a maximum operating frequency of
20 kHz. For alloy tuning purposes, the ability to fabricate and to test
small-scale samples may be highly cost efficient. Small sized sam-
ples—with thickness of ˜50 μm—can be tested on a vibratory based
fatigue tester (schematic diagram illustrated in Fig. 7 (top) [202,203].
Developed at the Los Alamos National Laboratory, this tester utilizes
samples that are of the thin-film (film thickness of about 50 μm) can-
tilever type. Under normal testing conditions, the bimorph piezoelectric
actuator drives the vibration of the sample at its resonant frequency
(Fig. 7 (bottom left)). The resonant frequency of a sample can be cal-
culated using linear elastic beam theory, i.e.
EI
ωn = βn 2
mL4 (4)
where ωn is the angular frequency, βn is a vibration-mode specific
constant (e.g., β1 = 1.875), E is the Young’s modulus of the sample, I is
the second moment of area of the cross section, m is the sample’s mass,
L is the length of the sample. The measured frequencies agree well with
Eq. (4) (Fig. 7 (bottom right)). The fatigue tests are feedback loop
controlled, i.e. the excitation frequency had to be constantly adjusted so
that the vibration amplitude is maintained at the desired level. Previous
studies have shown that when a critical shift in resonance frequency of
10 Hz is reached, fatigue cracks have formed and penetrated a sub-
stantial portion of the sample’s cross-section [202,203]. This frequency
shift may be used as a failure criterion.

7
S. Shao, et al. Additive Manufacturing 29 (2019) 100779

Fig. 8. A flow chart summarizing the existing literature (with references in blue) pertaining to the Model-Make-Measure-Verify approach in the efficient design of Ni-
superalloys.

In the verify stage, the information obtained from the “measure” cracks.
step, i.e. effect of composition, microstructure, and loading frequency, The operation of PSBs produces intrusions/extrusions on the surface
is necessary to verify the CGDD or higher length scale materials models. of metals, whose magnitude grow as a function of fatigue cycles
Using the validated model, the effects of microstructure and frequency [93,216,217]. At critical magnitudes, fatigue cracks initiate [216].
can then be quantitatively evaluated and enabling to establish a concise Therefore, any surface treatments that can remove or impede the for-
mathematical framework. mation of PSB or these surface features can extend the fatigue life of AM
For clarity, the literature reviewed in this overview article, per- parts. This has practical implications, as treatments can in principle be
taining to the stages of model make and measure, has been summarized developed and applied to existing AM parts in a non-destructive manner
in Fig. 8. to prolong their service life. Research activities in this regard is there-
fore highly desirable. This section identifies three niche research di-
rections that may offer potential breakthroughs in the enhancement of
9. An outlook on future’s research directions in AM
fatigue life of existing AM parts:
The AM research community has long realized the detrimental ef-
(1) Surface re-polishing: Periodically polishing away the surface in-
fects of AM induced defects —e.g. porosity, surface roughness, textured
trusions/extrusions has been shown to be able to, essentially, pro-
and columnar microstructure, etc.— on the fatigue resistance of AM
long the fatigue life of a conventionally manufactured part in-
metals [12,13,204–206]. Significant research efforts have thus been
definitely [216–218]—given that the treatment is done before the
devoted into pertinent topics, namely, effects of porosity, surface
formation of fatigue cracks. For AM parts, due to the pore-related
roughness/machining, build direction [206–210]. Surface and/or near-
nature of intrusions/extrusions, conventional mechanical polishing
surface defects are generally responsible for the initiation of fatigue
would be infeasible. Instead, electro-polishing could be effective in
cracks regardless of the load regimes, i.e. LCF, HCF or VHCF
removing intrusions/extrusions formed within surface-connected
[2,5,36,47]. To account for the effects of these surface related defects,
pores. This method is apparently ineffective for near-surface-buried
linear elastic fracture mechanics-based models such as the Murakami
pores.
model [211], has been adapted to predict the HCF fatigue resistance
(2) Surface hard coatings: Various ceramic-based hard surface coat-
with success [212–215]. Detrimental effects of surface roughness due to
ings have been applied on conventionally manufactured metals and
the AM process can be eliminated by AM near-net-shaping followed by
were shown to effectively inhibit the localized slip activities asso-
light machining. However, surface machining could also expose in-
ciated with PSBs [219]. Improvements in fatigue resistance is more
ternal pores to the surface-connected or near-surface-buried conditions.
pronounced in the HCF regime, as the higher loading amplitudes
Surface connected pores are preferential crack initiation sites due to the
under LCF tend to crack the ceramic coatings and leads to rapid
associated stress concentrations [211]. Near-surface-buried pores could
initiation of fatigue cracks [219]. Unique opportunities exist when
develop into surface-connected pores when the material ligament be-
applying nano-multilayered coatings to AM materials to sub-
tween the pore and the free surface fails [209,211]. The crack initiation
stantially improve both LCF and HCF strengths. These coatings,
mechanism may depend on the shape of the pores, i.e. the spherical
including metal/metal and metal/ceramic types, have hardness
pores leads to the accelerated formation of PSBs and therefore cracks,
comparable to ceramic hard coatings but with significantly higher
while the lack-of-fusion pores with sharp edges—smallest edge radius
ductility, thanks to the plastic co-deformation capabilities enabled
of curvature observed was ˜40 nm [13]—may serve as pre-existing

8
S. Shao, et al.
by the nano-multilayered architecture [167,220].
(3) Heat treatments (HT): The dislocation structures in PSB comprise
multipolar edge dislocations, which is thermally unstable. The PSBs
can be easily destroyed under recovery HT. For instance, PSBs in
single crystal Cu can be completely removed after recovery at
T = 0.44 Tm for 120 min [221]. Combining recovery HT with the
previous surface re-polishing and/or surface hard coatings may
offer substantial improvement to AM parts in service.
10. Summary
In this article, an overview of the literature relevant to the objective
of AM enabled, accelerated design of Ni-alloys for optimized high-cycle
and very-high-cycle fatigue performance is presented with identifica-
tion of the key knowledge gaps. The ultrasonic fatigue testing was
discussed as one of the key enabling technologies to achieve this ob-
jective, in light of their recent development and gain of popularity.
Achieving this objective demands fundamental understanding of the
effects of microstructure, composition, and test frequency on the op-
eration of dislocation arrays and, in turn, fatigue damage accumulation
of AM Ni-alloys, which is largely lacking at present. Overcoming these
knowledge gaps requires a systematic effort to address the complete
life-cycle of AM Ni-alloys—including computation-guided alloy design,
custom alloy powder synthesis, laser AM, comprehensive materials
characterization, accelerated in-situ/ex-situ fatigue testing, and ex-
perimental model validation.
Disclaimer
This report was prepared as an account of work sponsored by an
agency of the United States Government. Neither the United States
Government nor any agency thereof, nor any of their employees, makes
any warranty, express or implied, or assumes any legal liability or re-
sponsibility for the accuracy, completeness, or usefulness of any in-
formation, apparatus, product, or process disclosed, or represents that
its use would not infringe privately owned rights. Reference herein to
any specific commercial product, process, or service by trade name,
trademark, manufacturer, or otherwise does not necessarily constitute
or imply its endorsement, recommendation, or favoring by the United
States Government or any agency thereof. The views and opinions of
authors expressed herein do not necessarily state or reflect those of the
United States Government or any agency FA R&D Special TC NOVE-
MBER 2017- FF Page 4 of 12 thereof.
Acknowledgements
This material is based upon work supported by the U.S. Department
of Energy, Office of Science,Office of Basic Energy Sciences, under
Award Number DE-SC0019378. SS, SG, and WJM are also partially
supported by the NSF EPSCoR Consortium for Innovation in
Manufacturing and Materials (CIMM) program (grant number # OIA-
1541079). This work was performed, in part, at the Center for
Integrated Nanotechnologies, an Office of Science User Facility oper-
ated for the U.S. Department of Energy (DOE) Office of Science. Los
Alamos National Laboratory, an affirmative action equal opportunity
employer, is managed by Triad National Security, LLC for the U.S.
Department of Energy’s NNSA, under contract 89233218CNA000001.
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