crystals

Article
Analysis of Microstructure and Mechanical Properties in
As-Built/As-Cast and Heat-Treated Conditions for IN718 Alloy
Obtained by Selective Laser Melting and Investment
Casting Processes
Juan Carlos Pereira 1, *, Jon Aranzabe 1 , Mari Carmen Taboada 1 , Noelia Ruiz 2 and Pedro Pablo Rodriguez 2

1 LORTEK Technological Centre, Basque Research and Technology Alliance (BRTA), Arranomendia Kalea 4A,
20240 Ordizia, Spain; jaranzabe@lortek.es (J.A.); mctaboada@lortek.es (M.C.T.)
2 EIPC Research Centre, AIE, Torrekua 3, 20600 Eibar, Spain; nruiz@eipc.es (N.R.); prodriguez@eipc.es (P.P.R.)
* Correspondence: jcpereira@lortek.es; Tel.: +34-943-882-303

Abstract: In this work, new customized heat treatments for selective laser melted (SLM) parts in
IN718 alloy were analyzed. This was done through the evaluation of the mechanical properties
and advanced characterization of the phases and microstructure obtained in as-built condition and
after the application of standard and tailored heat treatments. The microstructure and mechanical
properties were compared and discussed with results reported in the literature. Finally, strengthening





 mechanisms of IN718 alloy processed by SLM and its differences with mechanisms that occur in
Citation: Pereira, J.C.; Aranzabe, J.; investment casting were analyzed. Both processes generate quite different microstructures, invest-
Taboada, M.C.; Ruiz, N.; Rodriguez, ment casting is composed mainly by a dendritic structure, and SLM is characterized by columnar
P.P. Analysis of Microstructure and and cellular structures with very thin cells. Due to the fine and homogeneous microstructure ob-
Mechanical Properties in tained from SLM processing and its specific strengthening mechanisms, it is not necessary to apply
As-Built/As-Cast and Heat-Treated homogenization and solution stages as in standard heat treatment used for this type of alloy in
Conditions for IN718 Alloy Obtained casting or wrought. The pre-heating and process parameters selected, in combination with a direct
by Selective Laser Melting and stepped aging (at 720 ◦ C/620 ◦ C), provide the material with its best mechanical properties, which are
Investment Casting Processes.
superior to those obtained by standard heat treatment (AMS 5383F) applied to investment casting of
Crystals 2021, 11, 1196. https://
IN718 alloy.
doi.org/10.3390/cryst11101196

Keywords: IN718 alloy; selective laser melting; investment casting; heat treatment; mechanical properties
Academic Editors: Pan Wang,
Takayoshi Nakano and Jiaming Bai

Received: 8 September 2021

Accepted: 29 September 2021
1. Introduction
Published: 2 October 2021 The nickel-based alloy Inconel 718 (IN718) is of high interest in the aeronautic,
aerospace, and oil & gas sectors, due to its good behavior at medium to high temper-
Publisher’s Note: MDPI stays neutral ature applications [1] where creep, corrosion, and heat resistance are needed [2]. It is
with regard to jurisdictional claims in also a key solution for hot structural applications, and its use is increasing day to day [3].
published maps and institutional affil- Additionally, laser-based additive manufacturing (AM) technologies are maturing apace to
iations. become alternatives to conventional manufacturing routes. These niche sectors demand
high performance components with adequate mechanical properties [4]. Recently, new
applications of hybrid manufacturing combining SLM with laser metal deposition (LMD)
and machining showed high potential and are promising for the aeronautic and aerospace
Copyright: © 2021 by the authors. sectors [5]. This type of hybrid manufacturing approach allows to obtain near-net-shape
Licensee MDPI, Basel, Switzerland. parts with reduced post-processing steps and lower buy-to-fly ratios.
This article is an open access article The aeronautical sector was one of the last sectors to adopt metal AM even with serial
distributed under the terms and production. According to the Wholers report, this industrial sector experienced a growth
conditions of the Creative Commons of 4.3% in 2015 and is the second largest sector in additive manufacturing, representing
Attribution (CC BY) license (https:// around 16% of the global market [6]. The 2018 Wholers report concludes that the 3D
creativecommons.org/licenses/by/ additive manufacturing industry increased by 21% to a total of $7 trillion in 2017, while the
4.0/).

Crystals 2021, 11, 1196. https://doi.org/10.3390/cryst11101196 https://www.mdpi.com/journal/crystals

Crystals 2021, 11, 1196 2 of 23

2019 Wholers report forecasts a growth of $35.6 trillion in the 3D additive manufacturing
industry by 2024 [7].
Metal AM offers a large number of very interesting advantages for the aeronautical
sector such as the light weighting of the components [8], consequent reduction in fuel
consumption, design freedom (possibility of creating complex shapes combining structural
optimization with topological optimization) [9], reduction of the purchase price, reduc-
tion in buy-to-fly ratio for large parts, simplification of the assembly process, reducing
time to market, etc. Therefore, research in process development with AM technologies
has increased.
Investment casting is a metal casting process. The process uses wax as a material
for the pattern. These patterns are subsequently coated with a ceramic shell in the form
of an investiture to generate a non-permanent mould with an upper opening through
which the wax is first removed, and whose hollow inner section serves as a mould or metal
container; this allows faithful copies of the original model to be made by metal casting.
The investment casting process has the following advantages: (1) narrow tolerances and
good dimensional accuracy; (2) good surface finish, better, in general, than traditional
casting methods; (3) ability to obtain complex geometries and thin wall thickness (around
1 mm); and (4) design flexibility. Both large and small pieces can be cast, although, of
course, within limits. Among the limitations of the process, it is worth highlighting the
following: (1) limitation in terms of size and weight of the parts, and (2) limitation in
terms of mechanical characteristics, since the molten metal is cast into a preheated mould.
This makes the cooling process slow, which generates large grain structures and, therefore,
mechanical properties (especially elongation) are worse compared to the ones of parts
manufactured by other processes, requiring a specific heat treatment to improve them. In
the specific case of nickel-based superalloys, the melting and casting processes, as well as
the subsequent thermal treatments, are performed under vacuum conditions, which makes
the process technologically more complex, consuming large amounts of energy, and the
associated costs increase.
The casting industry is following the evolution of metal additive manufacturing
technologies, and the SLM process in particular is being closely followed, since the devel-
opment of this technology and the latest advances can affect foundry in different ways.
SLM can be an alternative for the manufacturing of brackets, nozzles, tools, and moulds
with improved functionality, and on the other hand, AM can be a real alternative for the
manufacturing of certain types of complex parts and components in short series. The use
of this technology for direct production of functional parts is increasing, beyond its use to
obtain prototypes or casting models.
IN718 is a precipitation strengthening nickel-based alloy. The microstructure con-
sists of face-centered cubic (FCC) supersaturated solution matrix strengthened by γ0 -
Ni3(Nb,Ti,Al) and γ”-Ni3Nb. Other undesired phases such as laves phases, δ phases,
carbides (Cx), and nitrides (TiN) could be found in their microstructure in the as-built and
heat-treated conditions [2,10–12]. The strengthening effect of this alloy is given by the
precipitation of γ0 and γ” phases. The γ0 phase is a matrix-coherent cubic phase with a
spherical size around 20 nm, while γ” is a tetragonal metastable phase with morphology
of thin ellipsoidal discs. These phases precipitate from the supersaturated solid solution
during the double aging stage heat treatment, γ0 in the range of 621 ◦ C to 649 ◦ C, and γ”
in the range of 718 ◦ C to 760 ◦ C. The effectiveness of the double aging depends on the
Nb concentration and its distribution in the matrix, on the Al/Ti ratio [11] to optimize the
mechanical properties, and the relationship between them. Their morphology must be
taken into account independent of the manufacturing route of the IN718 alloy [11].
Additionally, Laves and δ phases are usually present in IN718 microstructure. The δ
phase is a Ni3Nb orthorhombic phase with Nb content between 6–8% (wt.%). It is formed
in the range of 650 ◦ C to 980 ◦ C. It is also formed from γ” phase in overaging [2,11,12]. The
Laves phases are hexagonally close-packed (Ni,Fe,Cr)2 (Nb,Mo,Ti) phases with a Nb content
Crystals 2021, 11, 1196 3 of 23

between 10–12% (wt.%) and hexagonally close-packed structure. According to different

authors, these phases are detrimental to ductility, and fatigue and creep resistance [3,11,13].
To achieve the required mechanical properties, it is necessary to carry out a thermal
treatment after SLM and casting processes. This treatment seeks to dissolve the undesired
phases and homogenize elements such as Ti, Nb, and Al in the matrix to promote the
precipitation of γ0 and γ”. In addition, with the thermal treatment it is possible to relieve
the stresses generated during the rapid cooling produced in SLM processing. That is the
main reason to develop and study new tailored heat-treatments for IN718 parts produced
with metal additive manufacturing.
The aim of this work is to analyze and compare the microstructure and mechanical
properties of IN718 alloy obtained by selective laser melting and investment casting pro-
cesses, in as-built/as-cast condition and under different heat treatments. The knowledge of
the strengthening mechanisms and aging response of IN718 SLM alloy and their correlation
with mechanical properties will allow the scientific and industrial community to have a
better understanding of the mechanical behavior for this alloy obtained by laser-based
additive manufacturing technique. Also, the comparison will be useful for future analysis
of whether a material manufactured by SLM can be an alternative to the industrial casting
process for commercial nickel-based alloys available to date, and for aeronautical applica-
tions at medium to high temperature where it could be economically viable, in particular,
for short production of geometrically complex parts with improved functionalities.

2. Materials and Methods

For the SLM process, IN718 gas atomized pre-alloyed powders were studied in detail
to ensure their flowability, spherical morphology, low internal porosity level, and chemical
composition in an initial benchmarking of four commercial powders from different suppli-
ers. Finally, IN718 powder manufactured by CARPENTER Additive (UK) was selected,
in particular the CT PowderRange IN718F grade powder, which has a specified particle
size distribution of 10–45 µm. The chemical composition of this powder is given in Table 1;
it fits within the classification of a nickel-based alloy of AMS 5596M type equivalent to
ASTM B670 and/or UNS N07718 Alloy. Particle morphology and microstructure were
observed in a Zeiss Ultra Plus field emission scanning electron microscope (FESEM). The
percentage of relative humidity present in the received powders was measured, as well
as the flowability of the particles (Hall Flowmeter Funnel according to ASTM B213-17)
and apparent density (according to ISO 3923-1). Internal porosity was also quantified
by image analysis taking 10 micrographs of the powder at 200X magnification. For the
porosity evaluation, 1500 particles were considered more or less. Particle size distribution
was measured taking into account around 14,000 particles.

Table 1. Chemical composition of IN718 powder used in SLM process (certificate for batch PR100026,
Carpenter Additive).

Elements and Chemical Composition Range (wt.%)

Cr Fe Nb + Ta Al Ti Si Mo Co C O Ni
19.30 18.24 4.93 0.49 0.96 0.03 3.00 0.04 0.03 0.02 52.96

Figure 1a summarizes the main SLM process parameters while Figure 1b shows the
axes and build direction (perpendicular to the build platform) as well as the scan pattern
strategy for reference in this work. The key parameters involved in SLM process are: laser
power P (W), focused spot diameter D (µm), scanning speed V (mm/s), distance between
tracks or hatch distance h (mm), layer thickness t (mm), and pre-heating temperature of
the chamber and build platform T (◦ C). The energy density E (J/mm3 ) that contributed to
a volume of material melted, is derived from some of these process parameters, and can be
 Crystals 2021, 11, 1196 4 of 24
Crystals 2021, 11, 1196 4 of 24

Crystals 2021, 11, 1196 4 of 23

the chamber and build platform T (°C). The energy density E (J/mm3) that contributed to
the chamber and build platform T (°C). The energy density E (J/mm3) that contributed to
a volume of material melted, is derived from some of these process parameters, and can
a volume of material melted, is derived from some of these process parameters, and can
be calculated using Equation (1), as it is a specific and very important parameter in the
be calculated using Equation (1), as it is a specific and very important parameter in the
SLM process
calculated development.
using Equation (1), as it is a specific and very important parameter in the SLM
SLM process development.
process development. 𝑃
P𝑃
E𝐸𝐸
=== 𝑉. ℎ. 𝑡
(1)
(1)
V𝑉.·hℎ.
·t 𝑡

Figure 1.Main
Mainparameters
parametersand
andaxes
axesininSLM
SLMprocess:
process:(a)
(a)parameters
parametersdenoted
denotedininone
onelayer
layerand
and(b)
(b)axes,
axes,build
builddirection,
direction, and
Figure 1. Main parameters and axes in SLM process: (a) parameters denoted in one layer and (b) axes, build direction, and
scan pattern strategy used for layers in SLM samples.
scan pattern strategy used for layers in SLM samples.

Forthis
For thisstudy,
study,the thelaser
laserpower
powerwas was212.5212.5W, W,andandthe
theapplied
appliedpreheating
preheatingtemperature
temperature
For this study, the laser power was 212.5 W, and the applied preheating temperature
on the
on the build
the build platform
build platform
platform was was
was 170 170 ◦
170 °C,°C, which
C, which
which was was selected
was selected
selected to to minimize
to minimize
minimize the the residual
the residual stresses
residual stresses
stresses
on
with thermal
with thermal origin,
thermalorigin, reducing
origin,reducing in
reducingininturn turn
turn the
the geometric
geometric distortions
distortions in the
in theprinted
printed part and the
with the geometric distortions in the printed partpart
andand
the
need
the needfor a
for greater
a thermal
greater thermalinputinputfor the
for selective
the melting
selective meltingof the
of particles.
the This
particles. also
This pro-
also
need for a greater thermal input for the selective melting of the particles. This also pro-
motes thethe
promotes characteristic
characteristic fine microstructure obtained and contributes to achieve the best
motes the characteristic fine fine microstructure
microstructure obtained
obtained and and contributes
contributes to achieve
to achieve the
the best
mechanical properties in the as-built condition. The The
partsparts
werewere manufactured using a Ren-
mechanical properties in the as-built condition. The parts were manufactured using a Ren-a
best mechanical properties in the as-built condition. manufactured using
ishaw RenAM
Renishaw RenAM 500Q Selective Laser Melting system. This machine is equipped with four
ishaw RenAM 500Q500Q Selective
Selective LaserLaserMelting Melting
system.system.
This This
machine machine is equipped
is equipped with with
four
Ytterbium
four Ytterbium fiberfiber
lasers (IPG(IPG
lasers Photonics,
Photonics, Oxford,
Oxford,MA,MA, USA) of 500
USA) of W each,
500 W working
each, in con-
working in
Ytterbium fiber lasers (IPG Photonics, Oxford, MA, USA) of 500 W each, working in con-
tinuous
continuous wave operation mode. The laser beams were focused to a diameter of around 80 µm
tinuous wavewave operation
operation mode. mode. The beams
The laser laser beams were focused
were focused to a diameter
to a diameter of aroundof around
80 µm
with
80 µm awith
Gaussian
a shapeshape
Gaussian and theand build
the chamber
build operates
chamber with awith
operates protective
a atmosphere,
protective with
atmosphere,
with a Gaussian shape and the build chamber operates with a protective atmosphere, with
0.2%0.2%
with beingbeing
the maximum
the maximum oxygen oxygenallowable during
allowable manufacturing
during manufacturing of theofparts.
the A linear
parts. A
0.2% being the maximum oxygen allowable during manufacturing of the parts. A linear
stripestripe
linear scan strategy was used
scan strategy with with
was used stripestripe
rotation of 67°
rotation 67◦ between
of between layers, and and
layers, argon was
argon
stripe scan strategy was used with stripe rotation of 67° between layers, and argon was
usedused
was as protection
as protection gas. For
gas.tensile tests, cylindrical
For tensile samples
tests, cylindrical (12 mm(12
samples diameter and 105and
mm diameter mm
used as protection gas. For tensile tests, cylindrical samples (12 mm diameter and 105 mm
105 mm height)
height) were manufactured
were manufactured on theon the “Z-axis”
“Z-axis” (or build
(or build direction)
direction) and and on the
on the “Y-axis”
“Y-axis” (or
height) were manufactured on the “Z-axis” (or build direction) and on the “Y-axis” (or
(or perpendicular to build direction), as indicated in Figure
perpendicular to build direction), as indicated in Figure 1b, employing the optimum pro- 1b, employing the optimum
perpendicular to build direction), as indicated in Figure 1b, employing the optimum pro-
processing parameters
cessing parameters determined
determined following
following the the methodology
methodology explained
explained in Section
in Section 3.2,
3.2, with
cessing parameters determined following the methodology explained in Section 3.2, with
with the of
the aim aim of obtaining
obtaining samples
samples withwith minimum minimum porosity
porosity level,level,
free free of defects,
of defects, and and
withwith
ade-
the aim of obtaining samples with minimum porosity level, free of defects, and with ade-
adequate surface
quate surface quality.
quality. TwoTwobuild
buildplatforms,
platforms,similar similartotothe
the one
one shown in Figure Figure 2, 2,were
were
quate surface quality. Two build platforms, similar to the one shown in Figure 2, were
necessary
necessaryto toproduce
producethe thesamples
samplesused usedin inthis
thisstudy.
study.
necessary to produce the samples used in this study.

Figure2.2.View
Figure Viewofofcylindrical
cylindricalsamples
samplesobtained
obtainedfrom
fromSLM
SLMprocess.
process.“Z-axis”
“Z-axis”samples
samples(left,
(left,center
centerand
and
Figure 2. View of cylindrical samples obtained from SLM process. “Z-axis” samples (left, center and
on the
on the right
the right of
right of the
of the platform)
the platform) and
platform) and “Y-axis”
and “Y-axis” samples
“Y-axis” samples (interspersed
samples (interspersed with
(interspersed with vertical
with vertical specimens).
vertical specimens).
specimens).
on

The investment casting process was done in an industrial environment, in the casting
facilities of Eibar Precision Casting (EIPC) located in Eibar, Gipuzkoa, Spain. A wax
 afterwards, the mould was dewaxed in an autoclave to obtain the final mould in which
the casting was made. Ingots of Inconel 718 alloy were used for the casting, and the meas-
ured chemical composition is shown in the first row of Table 2. For comparison, the chem-
ical composition of the raw material in samples from SLM and for investment casting pro-
cesses were measured again, in order to evaluate differences in their composition and to
Crystals 2021, 11, 1196 5 of 23
check for potential evaporation of some elements. Obtained results are compiled in Table
2.It can be observed that no major differences were detected in the IN718 Powder and
SLM samples.
structure with 20 rectangular block samples (50 mm width, 10 mm thick, and 100 mm
Table
large)2.was
Chemical composition
produced (Figuremeasured in thestructure
3a). The wax raw materials
was and in the manufactured
shell-coated samples.
with ceramic slurry
composed of three primaryElements
layers andandfive backup
Chemical layers to obtain
Composition the mould
Measured (wt.%) (Figure 3b);
Sample the mould was dewaxed in an autoclave to obtain the final mould in which the
afterwards, Cr Fe Nb + Ta Al Ti Si Mo Co C* O Ni
casting was made.
Ingot 17.78Ingots
19.91of Inconel
5.30 718 0.60alloy0.92
were0.070
used for the casting,
3.00 and the
0.30 0.050 measured
0.03 52.03
chemical composition
Invest Cast is shown
18.10 19.98 4.80in the0.57
first row
0.94 of 0.120
Table 2.2.83
For comparison,
0.13 0.054 the0.03chemical
52.50
composition
Powder of the raw17.90
19.20 material in samples
4.96 0.47 from0.96 SLM and 2.99
0.062 for investment casting
0.12 0.036 0.02processes
53.30
were measured again,
SLM Y-axis 19.20 17.80 in order to
5.00 evaluate
0.46 differences in
0.96 0.058 3.01their composition and to check
0.13 0.035 0.02 53.40 for
potential evaporation
SLM Z-axis 19.40 18.00 of some elements.
4.94 0.47Obtained results
0.95 0.042 2.99 are compiled in Table 2.It
0.10 0.032 0.02 53.20 can be
observed that no major differences were detected in the IN718
* Measured with ICP analysis with an internal method based on ASTM E1019-18. Powder and SLM samples.

Figure 3.
Figure 3. View
View of
of the
themould
mouldandandblock
blocksamples
samplesobtained
obtainedfrom
frominvestment
investment casting process
casting in in
process IN718. (a) (a)
IN718. Mould in wax,
Mould in wax,
(b) mould with shell after cast, and (c) mould without shell with integrated casts.
(b) mould with shell after cast, and (c) mould without shell with integrated casts.

The differences
Table 2. Chemical composition in chemical
measured in the rawcomposition
materials andin
in the raw material samples.
the manufactured used for the two manu-
facturing routes are due to the fact that a higher content of Si is required as a grain refiner
Elements and Chemical Composition Measured (wt.%)
Sample for the investment casting process and lower content of Cr is needed for fluidity of liquid
Cr Fe Nb +the
metal; Ta rest of Al Ti
the alloy elements Si in a similar
are Mo proportion.
Co C* O Ni
Ingot 17.78 19.91 The
5.30 relative density
0.60 in SLM
0.92 as-built
0.070 samples
3.00 was measured
0.30 by image
0.050 analysis
0.03 after
52.03
Invest using an Olympus GX51 optical microscope. Five images of the worst areas in the cross-
18.10 19.98 4.80of the sample
section 0.57 at 100X
0.94 magnification
0.120 2.83 taken0.13
were 0.054
for the analysis. 0.03 52.50
Manufactured
Cast
Powder 19.20 17.90
samples
4.96
obtained by SLM0.96
0.47
and investment
0.062
casting
2.99
processes
0.12
were heat treated
0.036 0.02
through
53.30
three combinations of homogenization, solution, and double aging thermal treatments in
SLM
19.20 17.80 a high-vacuum
5.00 furnace.
0.46 The first heat
0.96 treatment
0.058 studied was
3.01 0.13 the standard
0.035 one;
0.02 the specific
53.40
Y-axis
conditions of each stage are defined by standards such as AMS 2774F [14], which apply to
SLM
19.40 18.00 4.94 0.47 0.95 0.042 2.99 0.10 0.032 0.02 53.20
Z-axis
* Measured with ICP analysis with an internal method based on ASTM E1019-18.

The differences in chemical composition in the raw material used for the two manu-
facturing routes are due to the fact that a higher content of Si is required as a grain refiner
for the investment casting process and lower content of Cr is needed for fluidity of liquid
metal; the rest of the alloy elements are in a similar proportion.
The relative density in SLM as-built samples was measured by image analysis after
using an Olympus GX51 optical microscope. Five images of the worst areas in the cross-
section of the sample at 100X magnification were taken for the analysis. Manufactured
samples obtained by SLM and investment casting processes were heat treated through
three combinations of homogenization, solution, and double aging thermal treatments
Crystals 2021, 11, 1196 6 of 23

in a high-vacuum furnace. The first heat treatment studied was the standard one; the
specific conditions of each stage are defined by standards such as AMS 2774F [14], which
apply to wrought or additively manufactured materials for use in primary structural
components. Another reference standard is the AMS 5383F standard [15], used for the
heat treatment of investment casting components with this alloy. The homogenization and
solution stages must be carried out in a high vacuum furnace to avoid oxidation and to
obtain clean and unalterable surfaces in terms of chemical composition and therefore obtain
fully finished parts after heat treatment (in real applications). For all treatments a heating
rate of 10 ◦ C/min and minimum vacuum level of 5 × 10−3 mbar was applied, and the
specific conditions for each stage of the heat treatments (standard and tailored/modified)
are detailed in Table 3. The specific conditions (temperature and time) for the solution
stage in TT1 were selected considering their potential impact on the microstructure and
mechanical properties of SLM samples. Partial recrystallization appears over 1130 ◦ C,
and the original dendritic microstructure could be replaced by recrystallized grains in
some regions [16]. It is not desirable to prolong solution stage 2 beyond 2 h (coarsening
of microstructure). In fact, other authors also reported a considerable volume (>50%) of
recrystallization after annealing SLM-fabricated specimen at 1160 ◦ C for 4 h [12].

Table 3. Conditions for solid homogenization, solution, and artificial aging heat treatments.

Standard (TT0) Modified HT 1 (TT1) Direct Aging (TT2)

Stage Cooling
Condition Temp (◦ C) Time (h) Temp (◦ C) Time (h) Temp (◦ C) Time (h)
1093 to
482 ◦ C
Homogenization 1093 ± 10 2 — — — —
<45 min, then
air cooling
Solution Air cooling 954 ± 10 1 980 ± 10 1.5 — —
Cool down to
620 ◦ C at 720 ± 10 8 720 ± 10 8 720 ± 10 8
Double aging 55 ± 8 ◦ C/h
Air cooled in
620 ± 10 8 620 ± 10 8 620 ± 10 8
static air

The reference conditions for each stage were taken from those defined for the standard
heat treatment (TT0), and considering the fine dendritic microstructure obtained in as-built
(SLM) with the pre-heating and process parameters used, the homogenization stage was
removed, and the temperature and time of solution stage were reduced and increased
respectively in the TT1. For TT2, the aim was to study only direct aging of the samples.
In summary, for the double-stepped aging stage, same conditions of the standard heat
treatment were used for all heat treatments in order to compare potential improvements
in the precipitation hardening mechanisms between the different combinations of heat-
treatment stages but keeping the double-stepped aging condition.
For microstructural evaluation, the samples were cut from tensile coupons and con-
ventional metallographic preparations were made, embedding the samples in resin to then
carry out a roughing with abrasive papers with different granulometry, and a final pol-
ishing with diamond particles in suspension. Manual chemical etching (for SLM samples
only) was carried out with Kalling Nº 2 reagent for 12 s. The first observations were made
on an Olympus GX71 light optical microscope with an image acquisition system via digital
camera. The micrographs were evaluated at different magnifications (100X, 200X and 500X).
For advanced microstructural evaluation, a Zeiss Ultra Plus FESEM microscope equipped
with X-Max Oxford Instruments system and x-ray silicon drift detector (SDD) of 20 mm2
was used to acquire high magnification micrographs (5000X to 25,000X) and to perform
semi-quantitative analysis of the chemical composition by energy dispersive spectroscopy
(EDS). Finally, X-Ray Diffraction (XRD) analysis was used to identify the crystallographic
Crystals 2021, 11, 1196 7 of 23

Crystals 2021, 11, 1196 7 of

phases and their evolution with the heat treatments. The XRD was performed on a Philips
X’Pert machine using monochromatic Cu–Kα radiation (λ = 0.15406 nm). The XRD patterns
were obtained in the range of 2θ from 20 to 90◦ and were analyzed using X’Pert Plus
Tensile tests and hardness measurements of all samples (as-built/as-cast and hea
software (PANalytical).
treated)
Tensile tests were performed
and hardness in a Zwick Roell
measurements ofZ100 testing machine
all samples and in an EmcoTest
(as-built/as-cast and heat- DuraSca
durometer, respectively. To conduct the uniaxial
treated) were performed in a Zwick Roell Z100 testing machine and in an EmcoTest tensile tests, a nominal capacity of 100 kN
DuraScan durometer, respectively. To conduct the uniaxial tensile tests, a nominal equipped
and a test speed of 0.0005–500 mm/min were used. In addition, it is capacity with a
extensometer with elongation to break reading, extensible
of 100 kN and a test speed of 0.0005–500 mm/min were used. In addition, it is equipped arms up to 300 mm, and a ca
ibrated length
with an extensometer with range (Lo) from
elongation 10 to reading,
to break 100 mm.extensible
All tensilearms test up
samples
to 300weremm, andmachined be
a calibratedfore the test
length with
range (Lo)rounded
from 10 sub-size
to 100 mm. geometry according
All tensile to the ASTM
test samples were E8M guidelines an
machined
before theintest
correspondence
with roundedwith UNE-EN
sub-size geometry ISO 6892-1
accordingstandards.
to the ASTM E8M guidelines
Vickers hardness
and in correspondence with UNE-EN was measured
ISO 6892-1on the transversal section of the tensile sample
standards.
heads.
Vickers The measurements
hardness was measured on were
the carried
transversal out section
according of theto tensile
the UNE-EN
samples’ ISO 6507-1 stand
heads.
ard. The scale
The measurements wereapplied
carried out wasaccording
HV0.5 (Load to the0.5UNE-EN
kgf and ISO time6507-1
15 s) and nine measuremen
standard. The
were
scale applied wasmade
HV0.5 in each
(Loadsample,0.5 kgf inand thetime
cross 15 section
s) and nineof the sample (Ø 10were
measurements mm),madein a matrix o
in each sample, in the cross
measurements section of
separated fromthe each
sample other(Ø10 mm),mm,
at 1.75 in a and
matrix of 1.5
even measurements
mm from each of th
separatedendsfromor each
edgesother
fixed at 1.75
by the mm, and even 1.5 mm from each of the ends or edges
diameter.
fixed by the diameter.
In the present work, a total of 48 uniaxial tensile tests were carried out, 4 samples pe
In thecondition
present work,
and 12 a total of 48 conditions
different uniaxial tensile weretests were carried
studied, and theout, mean4 samples
value and per deviatio
condition were
and 12calculated
different conditions were studied, and the mean value and
from the results obtained in four tests for each condition/process. Amon deviation were
calculatedthose,
from the results
samples wereobtained in four tests
manufactured for each condition/process.
by investment casting, SLM Y Axis Among and those,
Z Axis, and fo
samples wereeachmanufactured
of those conditions by investment
four different casting,
heat SLM Y Axis
treatment and Z Axis,
conditions wereand usedfor(as-cast/as-bui
each
of those conditions
TT0, TT1 and fourTT2).
different heat treatment conditions were used (as-cast/as-built,
TT0, TT1 and TT2).
3. Results
3. Results
3.1. Powder Characterization
3.1. Powder Characterization
The pre-alloyed IN718 alloy powder used in this work showed a spherical morpho
The pre-alloyed IN718 alloy powder used in this work showed a spherical morphol-
ogy (Figure
ogy (Figure 4a), typical 4a),
of typical
the gasof the gas atomization
atomization process. Afterprocess. Aftersize
particle particle size distributio
distribution
analysis, the results revealed that a cumulative
analysis, the results revealed that a cumulative 10% mass-volume of the particles had 10% mass-volume of the particles
a had
smaller diameter than 17.7 microns for the powder;
smaller diameter than 17.7 microns for the powder; 50% of the particles were smaller than 50% of the particles were smaller tha
23.5 microns; and a cumulative 90% mass-volume
23.5 microns; and a cumulative 90% mass-volume of the powder particles had a smaller of the powder particles had a smalle
diameter diameter
than 31.1 than 31.1 microns.
microns. Particleand
Particle shape shapesizeand size distribution
distribution (diameter)
(diameter) analysis analysis
of of th
powder shown in Figure 4b is very important for
the powder shown in Figure 4b is very important for the SLM process. Due to the typical the SLM process. Due to the typic
recoater
recoater system usedsystem used inbed
in powder powder
fusionbed fusion machines,
machines, fine granulometry
fine granulometry and regular and regular size
sizes
and shapes are required, and an adequate flowability of the powder determines the best the be
and shapes are required, and an adequate flowability of the powder determines
packing ofpacking
particlesofinparticles
the powder in thebed powder bed layer
layer before the before the laser melting.
laser melting.

Figurepre-alloyed
Figure 4. IN718 4. IN718 pre-alloyed
powder. (a)powder. (a) Morphology
Morphology of theinparticles
of the particles SEM imagein SEM image
(20 kV) and(20
(b)kV) and (b) granulometry
granulometry and and
distribution
distribution analysis. analysis.

Flowability is another important aspect in SLM processing. As mentioned before, th

recoater systems requires particles to flow properly for an adequate distribution of th
powder bed in the machines, and to achieve suitable packing (due to different particle
size and its morphology) and ensure a certain layer thickness, which may influence th
lack of fusion and other relevant defects after laser processing. The IN718 pre-alloye
Crystals 2021, 11, 1196 8 of 23

Flowability is another important aspect in SLM processing. As mentioned before, the

Crystals 2021, 11, 1196 recoater systems requires particles to flow properly for an adequate distribution of 8 ofthe
24
powder bed in the machines, and to achieve suitable packing (due to different particles
size and its morphology) and ensure a certain layer thickness, which may influence the
lack of fusion and other relevant defects after laser processing. The IN718 pre-alloyed
powder selected in this work has sufficient flowability (18.74 ± 0.25 s/50 g) measured at 22 °C
powder selected in this work has sufficient flowability (18.74 ± 0.25 s/50 g) measured at
according to ASTM B213-17 Method 1 [17]. On the other hand, the measurement of ap-
22 ◦ C according to ASTM B213-17 Method 1 [17]. On the other hand, the measurement
parent density provides information on possible internal porosities of the material, as well
of apparent density provides information on possible internal porosities of the material,
as its adequate
as well packing,
as its adequate which which
packing, is alsoisassociated with the
also associated withmorphology
the morphology and and
size size
of theof
particles.
the particles.
Internal
Internal porosity
porosity inin the
the cross-section
cross-section of of powder
powder particles
particles was
was also
also evaluated.
evaluated. TheThe re-
re-
sults of the porosity measurements show a low percentage of internal
sults of the porosity measurements show a low percentage of internal porosity: 0.10 ± 0.12%, porosity: 0.10 ±
0.12%, which results
which results in a particles
in a particles densification
densification of 99.9 ± of 0.12%.
99.9 ± 0.12%.
This is This is positive,
positive, since ac-
since according
cording to various authors [18–21], the internal porosity of pre-alloyed
to various authors [18–21], the internal porosity of pre-alloyed nickel-based powders nickel-based pow- is
ders is revealed later, after rapid solidification, as gas trapped in
revealed later, after rapid solidification, as gas trapped in SLM-manufactured parts. Since aSLM-manufactured
parts.
lower Since
internala lower internal
porosity porosity
of the particlesof translates
the particles to translates to a greater
a greater apparent apparent
density den-
(without
sity (without considering the morphology of the powder and its influence
considering the morphology of the powder and its influence on the packing of the particles on the packing
of the particles
during during theofmeasurement
the measurement of apparent
apparent density), density),
a starting powder a starting
with the powder
lowestwith the
internal
lowest
porosity internal
possibleporosity possible
is desirable is desirable
to minimize to minimize
the presence the presence
of pores of pores after
after solidification so-
in laser
lidification
melting. The in results
laser melting.
obtained The results
from obtained
internal fromare
porosity internal porosity
also related to are
thealso relatedap-
measured to
the measured apparent density 3
(4.18 ± 0.01 g/cc 3) with the method defined in the ISO 3923-1
parent density (4.18 ± 0.01 g/cc ) with the method defined in the ISO 3923-1 standard and
standard
using the and Hallusing the Hall
flowmeter flowmeter
funnel. In Figurefunnel.
5, imagesIn Figure 5, images
of internal of internal
porosity analysisporosity
(Figure
analysis
5a) as well (Figure
as EDS5a)microanalysis
as well as EDS microanalysis
with the chemical with the chemical
composition composition
of particles of parti-
analyzed for
cles
this analyzed
powder (Figurefor this5b),
powder
which(Figure
confirms5b),the
which confirmsofthe
composition composition
IN718 alloy (AMS of IN718
5383F),alloy
can
(AMS 5383F), can be observed.
be observed.

Figure 5. IN718
Figure 5. IN718 pre-alloyed
pre-alloyed powder.
powder. (a) OM micrographs
(a) OM micrographs of
of particle
particle cross-sections
cross-sections (200X)
(200X) arrows
arrows indicate
indicate the
the porosities
porosities
revealed.
revealed. (b) FESEM of powder particles, and (c) Measurements of chemical composition by EDS (1000X, 20 kV, ModeSE).
(b) FESEM of powder particles, and (c) Measurements of chemical composition by EDS (1000X, 20 kV, Mode SE).

3.2. Selective
3.2. Selective Laser
Laser Melting
Melting Process
Process
The SLM
The SLM processing
processing parameters
parameters windowwindow can can become
become wide, since the preliminary
optimization
optimization can be done
done for the hatch (or core) on thepart,
for the hatch (or core) on the part,asaswell
wellasasforfor
thethe
definition of
definition
the edge/contour of each layer (affecting the tolerances and final surface
of the edge/contour of each layer (affecting the tolerances and final surface finish). How- finish). However,
after initial
ever, trials trials
after initial with awith
design of experiments
a design (DoE)(DoE)
of experiments composed
composedof three hatchhatch
of three distances
dis-
(0.07, 0.09,
tances (0.07,and 0.11
0.09, mm),
and 0.11two
mm),lasertwopowers
laser (217.5
powers and 240 W),
(217.5 and and
240 four
W), anddifferent
four scanning
different
speeds (650,
scanning 750, (650,
speeds 850, and
750,950
850,mm/s),
and 950 themm/s),
rest of the
the rest
parameters were constant:
of the parameters werepreheating
constant:
◦ C, laser spot diameter at focal point of 80 µm, and a layer thickness
preheating temperature of 170 C, laser spot diameter at focal point of 80 µ m, and a layer
temperature of 170
of 60 µm of
thickness in60
order to order
µ m in obtain tothe bestthe
obtain balance between
best balance surface
between finish,finish,
surface process time,time,
process and
and resolution. Recently published studies conclude that a combination of 200–285 W and
resolution. Recently published studies conclude that a combination of 200–285 W and
aa scanning
scanning speed
speed ofof 960–1000
960–1000 mm/s generates good
mm/s generates good material
material densification
densification [22] [22] and
and the
the
best mechanical
best mechanical properties
properties in in IN718
IN718 samples
samples obtained
obtained byby SLM
SLM [23]. In our
[23]. In our work,
work, aa similar
similar
trendwas
trend wasevidenced,
evidenced,and andgood
good results
results in in
thethe densification
densification of the
of the material
material werewere achieved.
achieved. Fig-
Figure 6 shows the evolution of the resulting material density in
ure 6 shows the evolution of the resulting material density in the hatch of cuboids (10 the hatch of cuboids
× 10 ×
10 × 10
(10mm × 10 mm3 ) manufactured
3) manufactured with thescanning
with the different different speeds
scanningandspeeds
hatchand hatch distances
distances derived
from the DoE. As it can be observed, material densification is higher for higherfor
derived from the DoE. As it can be observed, material densification is higher higher
scanning
speed values. In the same way, for higher scanning speed—as well as constant power,
hatch distance, and layer thickness—energy density is also lower (see Equation (1)), which
reduces the number of pores that appear due to gas trapped during solidification and its
Crystals 2021, 11, 1196 9 of 23

Crystals 2021, 11, 1196

scanning speed values. In the same way, for higher scanning speed—as well as constant
Crystals 2021, 11, 1196 power, hatch distance, and layer thickness—energy density is also lower (see Equation9(1)), of 24
which reduces the number of pores that appear due to gas trapped during solidification
vaporization
and its vaporization duringduring melting; melting; it is associated
it is associated to internal
to internal porosity
porosity and and humidity in th
humidity
in the powder der particles.
particles. After After evaluating
evaluating these these results,
results, a seta set of process
of process parameters
parameters forfor IN71
vaporization during melting; it is associated to internal porosity and humidity in the pow-
was selected.
IN718 alloy was selected. In Figure In Figure 7, we
we can see that low densification (mainly duegas-trapp
can see that low densification (mainly due to
der particles. After evaluating these results, a set of process parameters for IN718 alloy
to gas-trapped small lack oflack
and small fusion in the material)
of fusion occurredoccurred
in the material) for high laser energy
for high laserdensities
energy(above 65
was selected. In Figure 7, we can see that low densification (mainly due to gas-trapped and
3 ) combining
densities (above combining
65 J/mmhigh laser power high withlaserlowerpowerspeeds.
withThe bestspeeds.
lower results in Theterms
bestof materi
small lack of fusion in the material) occurred for high laser energy densities (above 65 J/mm3)
results in termssification
of material weredensification
achieved using were theachieved
lowest laser usingpowerthe lowest laser power
value considered (212.5 W) a
combining high laser power with lower speeds. The best results in terms of material den-
value considered ergy(212.5 W) and
density energy
between density
35–60 J/mm between
3, obtaining J/mm3 , densities
35–60material obtaininggreatermaterial than 99.95
sification were achieved using the lowest laser power value considered (212.5 W) and en-
densities greater than
final 99.95%. The
combination final
selected wascombination
a hatch selected
distance of was
0.11 mma hatch
and a distance
scanning of
speed of 850
ergy density between 35–60 J/mm3, obtaining material densities greater than 99.95%. The 3
0.11 mm and a scanning speed of 850 mm/s, resulting in an energy
resulting in an energy density of 37.9 J/mm and obtaining a material density of
3 density of 37.9 J/mm
final combination selected was a hatch distance of 0.11 mm and a scanning speed of 850 mm/s,
and obtaining a0.01%.material density
Other authors such±as0.01%.
of 99.97 Choi Other
et. al. authors
[24] andsuch Hakeemas Choi et al.
et. al. [24]
[25] reported d
resulting
and Hakeem in an energy
etvalues
al. [25]of density of
reported 37.9 J/mm
density values
3 and obtaining a material density of 99.97 ±
of 99.70% with 60–150 J/mm 3 and 99.50%
99.70% with 60–150 J/mm 3 and 99.50% with 50–70 J/mm 3, respectively, wh
0.01%.
with Other
50–70 J/mmauthors such as Choi
3 , respectively, which et.
areal.lower
[24] densification
and Hakeemvalues et. al. than
[25] the
reported
one density
obtained
lower densification values than the one obtained in this work. It is interesting to hi
values
in of 99.70%
this work. It is with 60–150
interesting toJ/mm
3 and 99.50% with 50–70 J/mm3, respectively, which are
highlight thatforthetheenergy density used for the best densified
that the energy density used best densified sample is lower than the range ex
lower densification
sample is lowerinthan values
the rangethanexplored
the one obtained in this work.
in the mentioned works.It isFinally,
interesting to highlight
the parameters
the mentioned works. Finally, the parameters for the contour were also optimized
that the energy
for the contouraweredensity used for the best densified sample is lower than the range explored
focusalso optimized
offset in the fillusing
contour, a focustakingoffset
as aincriterion
the fill contour,
not onlytaking as a densifi
the greatest
in the mentioned
criterion not only works.
the Finally,
greatest the parameters
densification, but for
also the
thecontour
smallest were also
deviation optimized
of the using
edge’s
but also the smallest deviation of the edge’s surface, which will generate a better
a focus which
surface, offset inwillthe fill contour,
generate taking as aroughness
criterion not only thegeometries.
greatest densification,
roughness in acomplex
better surface
geometries. in complex
but also the smallest deviation of the edge’s surface, which will generate a better surface
roughness in complex geometries.

Figure 6. Evolution
Figure 6. of materialofdensity
Evolution as density
material a function
as aoffunction
scanningofspeeds forspeeds
scanning different
forhatch distance
different hatchand laser power.
distance
(a) Material density
and laser for 212.5(a)
power. W,Material
and (b) density
density evolution using
for 212.5 W, and0.11
(b) mm hatch
density distance.using 0.11 mm hatch
evolution
Figure 6. Evolution of material density as a function of scanning speeds for different hatch distance and laser power.
distance.
(a) Material density for 212.5 W, and (b) density evolution using 0.11 mm hatch distance.

Figure 7. Micrographs of the cross-section of SLM cuboids with different process parame
power: 240 W, speed: 650 mm/s, and hatch distance of 0.09 mm. (b) power: 212.5 W, speed: 85
Figure 7.7. Micrographs
Figure Micrographs of
and hatchof the
thecross-section
cross-section
distance ofofSLM
of 0.11 mm. SLMcuboids
cuboidswith
withdifferent process
different parameters.
process (a)
parameters.
power: 240 W, speed: 650 mm/s, and hatch distance of 0.09 mm. (b) power: 212.5 W, speed:
(a) power: 240 W, speed: 650 mm/s, and hatch distance of 0.09 mm. (b) power: 212.5 W, speed: 850 mm/s,
and hatch distance of 0.11 mm.
3.3. Investment
850 mm/s, and hatch Casting
distance of 0.11 mm.Process
TheProcess
3.3. Investment Casting investment casting process was carried out in an industrial environmen
the facilities of the company Eibar Precision Casting (EIPC). The wax patterns w
The investment casting process was carried out in an industrial environment using
jected in a vertical machine at 65 C. Then, the patterns were mounted in a recycl
the facilities of the company Eibar Precision Casting (EIPC). The wax patterns were in-
jected in a vertical machine at 65 C. Then, the patterns were mounted in a recycled wax
Crystals 2021, 11, 1196 10 of 23

3.3. Investment Casting Process

The investment casting process was carried out in an industrial environment using the
facilities of the company Eibar Precision Casting (EIPC). The wax patterns were injected in
a vertical machine at 65 ◦ C. Then, the patterns were mounted in a recycled wax structure
as previously shown on the left of Figure 3. Afterwards, the wax structure was shell coated
using robotic equipment with the following materials:
• For primary coatings, a slurry made of colloidal silica binder and zircon flour was
used. Then, the mould was stuccoed with zircon sand.
• For secondary coatings, a slurry made of colloidal silica binder and silica flour was
used. Then, the mould was stuccoed with silica sand.
Once the mould was dry, it was dewaxed in an autoclave with water vapor at 150 ◦ C
and a pressure of 9 bar. Then, the mould was fired and preheated at 1150 ◦ C prior to the
casting, whereas the molten material was poured at 1450 ◦ C. Both the IN718 melting and
the pouring processes were carried out under vacuum atmosphere. The mould was then
taken out from the vacuum furnace and cooled down at room temperature. The knockout
and sample cleaning operations were then carried out to obtain parts ready for thermal
treatment and subsequent machining post-processing.

4. Discussion
4.1. Comparison of Microstructures
In the SLM process, micrographs cross section with horizontal orientation (Y axis)
and build direction (Z axis) are shown. In the samples manufactured by SLM in as
built condition, both in the Y-axis and the Z-axis samples (Figure 8) a very fine cellular
microstructure typical of selective laser melting processes is observed, due to the rapid
solidification of fast laser material processing [2,11,12,26] and because of the high cooling
Crystals 2021, 11, 1196 rate (105 to 107 k/s) during the SLM process [24]. Columnar and cellular sub-structures 11 of 24
formed in the overlapping area (where re-melting occurs) are observed, while mainly
cellular sub-structures are present in the area of fusion inside the tracks.

Figure
Figure 8. Optical
8. Optical micrographs
micrographs forfor IN718
IN718 inin as-built/as-castand
as-built/as-cast andheat-treated
heat-treated condition.
condition. (a–d): SLM samples
(a–d) SLM samples in
in Y-axis,
Y-axis, (e–
h): SLM samples in Z-axis, and (i–l): Investment casting samples. (SLM samples are etched with Kalling Nº2 and invest-
(e–h) SLM samples in Z-axis, and (i–l) Investment casting samples. (SLM samples are etched with Kalling Nº2 and
ment casting samples only polished).
investment casting samples only polished).

The microstructure of the samples manufactured in both orientations is similar with

the only difference in the orientation of the grains and the re-melted and thermally af-
fected areas; therefore, FESEM images are shown only on the Y axis (Figure 9). The micro-
Crystals 2021, 11, 1196 11 of 23

The micrographs of Y axis samples (Figure 8a) show the cross section of the melt pool
tracks in the successive passes of the laser beam during layer-by-layer manufacturing. In
the cross section of the SLM samples manufactured in vertical orientation (Z axis of the
machine) shown in Figure 8e, the top view of the melt pool tracks in the successive passes
of the laser beam during the manufacturing of one or two layers (cross section not exactly
on one layer) is observed. The scanning strategy used (stripes with 67◦ rotation in each
layer) generates the direction changes observed in the laser beam trajectories. There are
fewer re-melted and thermally affected areas in the XZ plane, Figure 8a, than in the XY
plane. The differences observed in the microstructure (and also in their crystallography) on
each direction can directly affect the mechanical properties (anisotropy) that metal alloys
obtained by SLM usually present in their delivery state (as-built condition). In samples
manufactured in both orientations, a low level of porosity can be observed.
The microstructure of the samples manufactured in both orientations is similar with
the only difference in the orientation of the grains and the re-melted and thermally affected
areas; therefore, FESEM images are shown only on the Y axis (Figure 9). The microstructure
of these specimens is characterized by a very thin cell structure, with a dendrite arm spacing
of less than 1 µm and a fine precipitation in the grain borders (See Figure 9a,e). These
precipitates are rich in Niobium. According to Deng et al. [27] and Popovich et al. [28],
they are Laves precipitates. The formation and precipitation of Laves phase reduces the
Niobium content available for the constitution of γ0 and γ” precipitates [11,16,26,27],
Crystals 2021, 11, x FOR PEER REVIEW 12 so
of it
24
is important to control their formation to allow the adequate strengthening and subsequent
achievable mechanical resistance in the material.

Figure 9.
Figure 9. FESEM
FESEMmicrographs
micrographsatatdifferent magnifications
different magnificationsfor for
IN718 SLMed
IN718 in as-built
SLMed and heat-treated
in as-built conditions.
and heat-treated (a–d):
conditions.
SLM samples in Y-axis, and (e−h): SLM samples in Z-axis. (all samples etched with Kalling Nº
(a–d) SLM samples in Y-axis, and (e–h) SLM samples in Z-axis. (all samples etched with Kalling Nº2).2).

The microstructure
The microstructure observed
observed in in the
the samples
samples manufactured
manufactured by byinvestment
investment casting
casting in
in
as-cast-condition (Figure 10)
as-cast-condition 10) isisvery
verydifferent
differenttotothatthatseen
seen in in
as-built
as-builtSLMedSLMed parts. Invest-
parts. In-
ment casting
vestment samples
casting in as-cast
samples condition
in as-cast conditionshowshowa dendritic structure
a dendritic with with
structure an average spac-
an average
ing of the
spacing secondary
of the secondarydendritic
dendritic arms
arms of of
approximately
approximately5050µµm; m; this
this is
is the typical casting
casting
microstructurefor
microstructure forIN718
IN718alloy
alloy obtained
obtained with with slow
slow solidification
solidification speedspeed
[25].[25]. The micro-
The microstruc-
structure
ture is constituted
is constituted by gamma
by gamma nickelnickel
matrix, matrix, large Laves
large Laves (rich in(rich
Nb in andNbMo),
andand
Mo),delta
and
delta phases
phases of irregular
of irregular segregation
segregation in the interdendritic
in the interdendritic zones (see zones (see10),
Figure Figure
which 10),
is awhich
similaris
a similar microstructure
microstructure to thatby
to that reported reported by other
other authors [6].authors [6]. The segregation
The segregation of Nb and Mo of Nb and
during
the
Mocasting
duringprocess produces
the casting process a heterogeneity of these elements
produces a heterogeneity and elements
of these during solidification
and during
the laves and the
solidification delta phases
laves are formed
and delta phasesin arethe dendrites
formed in the[25]. Titanium
dendrites [25].nitrides
Titaniumwere also
nitrides
detected in specific zones.
were also detected in specific zones.
 delta phases of irregular segregation in the interdendritic zones (see Figure 10), which is
a similar microstructure to that reported by other authors [6]. The segregation of Nb and
Mo during the casting process produces a heterogeneity of these elements and during
solidification the laves and delta phases are formed in the dendrites [25]. Titanium nitrides
Crystals 2021, 11, 1196 were also detected in specific zones. 12 of 23

Figure 10.
Figure 10. FESEM
FESEM micrographs
micrographsfor forIN718
IN718 investment casting
investment in As-cast
casting and and
in As-cast heat-treated conditions.
heat-treated (a–d): Investment
conditions. casting
(a–d) Investment
samples at low magnification, and (e–h): Investment casting samples at high magnification. (samples not etched, only polished).
casting samples at low magnification, and (e–h) Investment casting samples at high magnification. (samples not etched,
only polished).
When applying the AMS standard heat treatment (TT0) in the SLM samples, the cel-
lularWhen
structure observed
applying in as-built
the AMS condition
standard disappears(TT0)
heat treatment and in
grain
the growth is observed
SLM samples, the
cellular structure observed in as-built condition disappears and grain growth is observed
due to the homogenization step of the heat treatment, as can be seen in Figure 9b,f. The mi-
crostructure analysis reveals bigger phases distributed in grain boundaries (see Figure 11).
These phases, according to their morphology and chemical composition, correspond to
delta phases in two morphologies: short-rod and needle shape, and Laves phases, which
were not dissolved in the homogenization step [29]. The presence of small sub-micrometric
Crystals 2021, 11, 1196 γ0 and γ” precipitates in the gamma nickel matrix can be appreciated although they 13 of are
24

not clearly distinguished due to their small size (nanometric range).

Figure11.
Figure FESEM
11.FESEM micrographfor
micrograph for IN718
IN718 alloy
alloy with
with standard
standard heat
heat treatment—TT0(polished
treatment—TT0 (polishedsample,
sample,
SESEmode).
mode).(a):
(a)SLM
SLMY-axis
Y-axissample
sampleand
and(b):
(b) the
the respective
respective x-ray
x-ray elemental maps through EDS.

InInthe
thecase
homogenization
of the samplesstep it is possible
manufactured bytoinvestment
dissolve acasting,
large part
it isofobserved
the Laves phases
that the
and due microstructure
dendritic to the high temperature of this step,
is more globular and thealsodissolution
Nb diffuses ofinthe
thesegregated
matrix, achieving
phases
precipitation
occurred of the
to a great deltabut
extent phase
notduring the subsequent
completely, since somesolution
remainingstage
Laveswhen theseare
phases phases
ob-
served and still remain in the microstructure (Figure 9b,f). The homogenization stage of
the microstructure is very important in the investment casting processing route to dissolve
these undesirable phases and to enhance the precipitation of gamma prime and double
gamma phases that reinforce the matrix of this material [33,34]. Laves phase and possible
Crystals 2021, 11, 1196 13 of 23

are formed at the grain boundaries. Previous research works [2,30] reported that with a ho-
mogenization step at 1080 ◦ C a uniform distribution of Nb is achieved, minimizing acicular
δ phase precipitation during the solution stage. Delta phase precipitates at temperatures
between 650 ◦ C and 980 ◦ C [31], so it does not precipitate during the homogenization stage
but could do it in the following stages of the thermal treatment. This precipitation is mainly
needle-shaped
Figure 11. FESEMand locatedfor
micrograph onIN718
the grain edges.
alloy with These
standard precipitates
heat treatment—TT0 have(polished
been observed
sample,
to mode).
SE prevent (a):grain growth
SLM Y-axis and and
sample dislocation sliding mechanism
(b): the respective x-ray elemental during
maps high temperature
through EDS.
exposure in IN718 alloy [2,25,32].
In
Inthe
thecase
caseofofthethesamples
samples manufactured
manufactured bybyinvestment
investment casting, it isitobserved
casting, thatthat
is observed the
the dendritic
dendritic microstructure
microstructure is more
is more globular
globular andandthethe dissolutionofofthe
dissolution thesegregated
segregated phases
phases
occurredto
occurred toaagreat
greatextent
extentbutbut not
not completely,
completely, since
since some
some remaining
remaining Laves Laves phases
phases are
are ob-
observed and still remain in the microstructure (Figure 9b,f). The
served and still remain in the microstructure (Figure 9b,f). The homogenization stage of homogenization stage
of the
the microstructure
microstructure is very
is very important
important in the in the investment
investment casting casting processing
processing route to
route to dissolve
dissolve
these these undesirable
undesirable phases and phases and to enhance
to enhance the precipitation
the precipitation of gamma of gamma
prime and prime and
double
double gamma
gamma phases thatphases that reinforce
reinforce the matrixtheofmatrix of this material
this material [33,34].
[33,34]. Laves Laves
phase andphase and
possible
possible
delta delta
phase arephase are also observed
also observed with the with
shapes theofshapes
needles of needles thus irregularly
thus irregularly shaped,shaped,
but al-
but always at the edges of the grain or in the vicinity of it (Figure
ways at the edges of the grain or in the vicinity of it (Figure 12), as in the sample manu-12), as in the sample
manufactured
factured by theby SLMtheprocess.
SLM process.

Figure
Figure 12. FESEM
FESEM micrographs
micrographs forfor IN718
IN718 alloy
alloy obtained
obtained by
by investment
investment casting.
casting. (a):
(a) with standard heat treatment—TT0
treatment—TT0
(polished sample). (b): the respective x-ray elemental maps through EDS.
(polished sample). (b) the respective x-ray elemental maps through EDS.

By eliminating the homogenization stage, in the so-called modified heat treatment

(TT1), a finer structure with smaller Laves and delta phases with a uniform distribution
was achieved in the case of SLM. This is due to the fact that, without the homogenization
stage, these phases do not dissolve. It is also appreciated that there is a higher delta phase
density but smaller size that could have formed, particularly for this heat treatment.
Previously, it was observed that the solution treatment at 980 ◦ C for 1 h without
homogenization stage was not sufficient to dissolve Laves phases present in the as-built
microstructure of SLM samples [2]. In addition, with the temperature being too low, there is
not enough driving force for Nb to diffuse and homogenize its concentration throughout the
gamma matrix, since this element easily segregates at the grain borders and interdendritic
regions, enhancing the formation of Laves (10–12 wt.% of Nb) and delta (6–8 wt.% of Nb)
phases. Due to this dissolution and diffusion phase, the delta phase precipitates in the
 mogenization and double aging treatment, thus avoiding, to a great extent, the precipita-
tion of the delta phase [10]. The delta phase is a detrimental phase on the mechanical
properties for two reasons: First, it consumes the Nb content, reducing the potential for
precipitation of ′ and ″, and second, the Laves phases are starting points for crack prop-
agation, affecting their structural integrity [32] and accelerating the failure in service.
Crystals 2021, 11, 1196 14 of 23
In the case of investment casting, the dissolution of the phases that were in the inter-
dendritic regions was not achieved and the traces of dendrites but with smaller interden-
dritic arms compared to the as-cast sample were observed. Laves phases of greater size
interdendritic
than those observed after the regions andof
application grain borders in
the standard the TT1 both
treatment, in acicular
appeared; and needle-like form
in addition,
(Figure
titanium nitrides were13), in addition
observed to remaining
together with theseLaves phase
phases, that did
as shown in not dissolve
Figure 14. [30].

Figure micrograph
Figure 13. FESEM 13. FESEM micrograph for IN718
for IN718 alloy alloy with
with modified modified
heat heat(polished
treatments treatments (polished
samples, (a) samples, (a): with TT1
Y-axis sample
Y-axis
(25,000X, left), andsample with TT1 (25,000X,
(b) the respective left), and
X-ray elemental (b): through
maps the respective X-ray elemental maps through EDS
EDS (right).
(right).
Other research works suggest eliminating the solution step and carrying out a homog-
enization and double aging treatment, thus avoiding, to a great extent, the precipitation of
the delta phase [10]. The delta phase is a detrimental phase on the mechanical properties for
two reasons: First, it consumes the Nb content, reducing the potential for precipitation of
γ0 and γ”, and second, the Laves phases are starting points for crack propagation, affecting
their structural integrity [32] and accelerating the failure in service.
In the case of investment casting, the dissolution of the phases that were in the
interdendritic regions was not achieved and the traces of dendrites but with smaller inter-
dendritic arms compared to the as-cast sample were observed. Laves phases of greater size
than those observed after the application of the standard treatment, appeared; in addition,
titanium nitrides were observed together with these phases, as shown in Figure 14.
After the double-stage aging heat treatment (direct aging, TT2), tracks and cellular
structures (similar to the ones found in as-built condition) were observed in the cross-
section of the SLM samples, not achieving a coarsening of the microstructure. The direct
double aging applied to the SLM samples does not substantially modify the fine den-
dritic structure obtained after processing (compared to the as-built condition observed
in Figure 9d). In addition to the hardening effect of the fine delta phase particles in the
interdendritic zones, the potential effect of phase precipitation could be in the gamma
nickel matrix itself. The presence of these precipitates can be intuited, but they are too
small (nanometric scale) to be correctly identified in FESEM micrographs. Small Cx-type
carbides and small titanium nitrides are also present in the TT2 microstructure (Figure 9h).
The investment casting samples treated with only the stepped aging stage present a
very similar microstructure to that observed in the as-cast samples without heat treatment
(Figure 10a), but with a smaller size of dendritic arms, where there are large delta phase
islands, accompanied in some areas, by irregularly shaped particles (Laves phase), formed
after solidification (Figure 10h).
Crystals 2021, 11, 1196 15 of 23
Crystals 2021, 11, 1196 15 of 24

Figure 14.
Figure 14. FESEM
FESEM micrograph
micrograph for
for IN718
IN718 alloy
alloy obtained
obtained by
by investment
investment casting.
casting. (a)
(a):with
withmodified
modified
heat treatment—TT1 (polished samples, SE mode), and (b): the respective X-ray elemental
heat treatment—TT1 (polished samples, SE mode), and (b) the respective X-ray elemental maps maps
through EDS.
through EDS.

AfterIdentification
4.2. Phase the double-stage aging heat treatment
and Evolution—XRD Analysis(direct aging, TT2), tracks and cellular
structures
To study(similar to the ones found
the crystallographic phase’s in as-built
presence condition) were observed
in the as-built/as-cast in the cross-
conditions and
section of the SLM samples, not achieving a coarsening of
their evolution with the heat treatments, a XRD analysis was performed. Figure 15 showsthe microstructure. The direct
double
the aging applied
diffraction to the SLM
pattern obtained forsamples doesconditions.
the different not substantially modify the fine
In the pre-alloyed powder dendritic
used
structure obtained after processing (compared to the as-built
for the SLM process, the principal phases are gamma and/or gamma prime: γ-Ni(Fe,Cr) condition observed in Figure
9d). In addition
and/or to the hardening
γ0 -Ni3 (Al,Ti). Similar phases effectareof the fine delta
detected bothphase
in SLMparticles in the interdendritic
and investment casting
zones, thesince
samples, potential 0
γ/γ /γ” effect of phase
have similarprecipitation
crystallography couldaccording
be in the togamma
the peak nickel matrixfor
intensity it-
self. The
each presence
phase. Phaseofdetection
these precipitates
in XRD technique can be intuited, but they
has limits: Onlyarecrystallites
too small (nanometric
larger than
scale)
10 nm toarebedetected
correctly [35]identified in FESEM
and it usually failsmicrographs.
to recognize phasesSmall Cx-type
presentcarbides
at less than and5%small
of
titanium nitrides are also present in the TT2 microstructure (Figure
mass fraction in the specimen. The existence of γ” is not well detected in the XRD pattern 9h).
due theTheoverlapping
investment casting of their samples
peaks with γ/γ0with
treated only
. There arethe
nostepped
evidentaging
peaksstage present
for delta anda
very similar
Laves phases, microstructure
perhaps due to that theirobserved in the as-cast
low volumetric fractionsamples
in thewithout heat treatment
alloys obtained with
(Figure
both 10a), but with
manufacturing a smallerbut
processes, size of dendritic
strong <111> and arms, where
<200> there arepeaks
diffraction large for delta
γ/γ 0 are
phase
islands, accompanied
observed in somestudied,
in all the conditions areas, byand irregularly shapedwith
it is consistent particles
XRD(Laves
patterns phase), formed
reported for
after solidification
IN718 SLMed samples (Figure 10h).authors [25,30,32,36].
by some
Li X. et al. [32] also detected the presence of delta <211> diffraction peak in SLM
4.2. Phase
samples Identification with
manufactured and Evolution—XRD
IN718 and directAnalysis aged, but no peak was detected in the as-built
condition, which
To study theleads us to think that
crystallographic the temperatures
phase’s presence inused by them in the double
the as-built/as-cast conditionsstepped
and
aging stage (higher than those used in this work) promoted the
their evolution with the heat treatments, a XRD analysis was performed. Figure 15 shows formation/modification of
the delta phase in detriment of the precipitation of strengthening phases (γ 0 /γ”), which
the diffraction pattern obtained for the different conditions. In the pre-alloyed powder
are
usednotfor
thethedesired
SLM precipitation kinetics for
process, the principal the SLM
phases are processing.
gamma and/or In this
gamma XRD prime:
analysis,-
the presence of delta and lave phases was not detected in
Ni(Fe,Cr) and/or ′-Ni3(Al,Ti). Similar phases are detected both in SLM and investmentthe patterns for the different
conditions studied.
casting samples, since /′/″ have similar crystallography according to the peak intensity
A slight shift
for each phase. Phase to the left is noticed
detection in XRD intechnique
the peaks hasof the as-built/as-cast
limits: samples,
Only crystallites which
larger than
is 0
10more evident
nm are detected in peaks <220>
[35] and and <311>
it usually forrecognize
fails to γ/γ , andphases
this shows
presentthatatthere is indeed
less than 5% of
a change in the crystallography of the present phases, and the only possibility is the
mass fraction in the specimen. The existence of ″ is not well detected in the XRD pattern
potential dissolution of the minority delta and Laves phases (in the case of TT0 and TT1)
due the overlapping of their peaks with /′. There are no evident peaks for delta and
and subsequent precipitation of the strengthening phases of these alloys (in the TT0, TT1,
Laves phases, perhaps due to their low volumetric fraction in the alloys obtained with
and TT2 heat treatments).
both manufacturing processes, but strong <111> and <200> diffraction peaks for /′are
observed in all the conditions studied, and it is consistent with XRD patterns reported for
IN718 SLMed samples by some authors [25,30,32,36].
 mass fraction in the specimen. The existence of ″ is not well detected in the XRD pattern
due the overlapping of their peaks with /′. There are no evident peaks for delta and
Laves phases, perhaps due to their low volumetric fraction in the alloys obtained with
both manufacturing processes, but strong <111> and <200> diffraction peaks for /′are
observed in all the conditions studied, and it is consistent with XRD patterns reported for
IN718 SLMed samples by some authors [25,30,32,36].
Crystals 2021, 11, 1196 16 of 23

Figure 15. X—Ray

Figure 15.diffraction patterns
X—Ray diffraction patternsof IN718
of IN718 powder,
powder, SLM,
SLM, and and investment
investment casting samples.casting samples.

4.3. Comparison of Mechanical Properties

For the testing of mechanical properties, cylinders (in the case of SLM) and rectangular
plates (in the case of investment casting) were manufactured, from which cylindrical tensile
samples were obtained after cutting, machining, and turning. As for SLM samples, they
were manufactured in two different orientations, horizontal (Y axis) and vertical (Z axis).
The aforementioned heat treatments (Table 3) were applied to both samples manufactured
by means of SLM and investment casting, so that four samples of each condition were
tested. After performing tensile tests, some sections of the samples were cut to measure the
micro hardness of the material.
The summary of results obtained from the tensile tests for SLM samples is shown in
Table 4. The results were calculated as the mean value of three tests performed (out of four).
The value obtained in the fourth test was taken into account because of different reasons,
such as problems during the test itself (jaw slips or extensometer displacement) and/or big
deviations in results compared to other samples tested in the same condition.
Table 4. Summary of mechanical properties for IN718 alloy obtained by SLM.

SLM SLM SLM SLM SLM SLM SLM SLM

Process
Y Axis Z Axis Y Axis Z Axis Y Axis Z Axis Y Axis Z Axis
Condition As-Built TT0 TT1 TT2
σy (MPa) 756.1 ± 2.7 638.9 ± 2.0 1243.1 ± 10.6 1235.6 ± 19.7 1300.1 ± 4.9 1236.7 ± 10.7 1420.1 ± 42.3 1267.6 ± 8.2
UTS (MPa) 1054.5 ± 1.9 1001.5 ± 4.3 1445.9 ± 2.7 1414.9 ± 6.5 1508.2 ± 4.2 1447.6 ± 9.5 1567.4 ± 40.5 1464.9 ± 4.2
E (GPa) 201.0 ± 2.7 185.9 ± 2.0 211.1 ± 4.1 208.2 ± 6.5 207.3 ± 4.9 204.5 ± 6.6 212.3 ± 1.7 207.5 ± 5.8
ε (%) 30.1 ± 0.2 31.1 ± 0.6 18.9 ± 0.4 17.6 ± 2.2 17.9 ± 0.5 18.0 ± 0.1 15.7 ± 0.3 19.1 ± 1.2

Figure 16 shows the high strength that was obtained in the IN718 Alloy with the
SLM process; in particular, in the as-built condition, the mechanical properties obtained
for the horizontal and vertical samples are slightly higher than those reported by some
other authors. For instance, Li et al. [37] reported as-built yield strength and UTS values
of 590 ± 5 MPa and 935 ± 16 MPa respectively. In the case of Zhang et al. [30], results
obtained in this work are below the ones reported. On the other hand, anisotropy is
observed between the SLM samples manufactured with vertical and horizontal disposition
for this condition, reaching differences in as-built condition of around 5.3% in the maximum
resistance, 18.3% in the yield strength, and 3.3% in the elongation until rupture. The
horizontal samples (Y-axis) were those that presented the highest resistance with the lowest
ductility. Although it is noteworthy that a low variability in the results was evidenced
 thors. For instance, Li et al. [37] reported as-built yield strength and UTS values of 590 ± 5
MPa and 935 ± 16 MPa respectively. In the case of Zhang et al. [30], results obtained in this
work are below the ones reported. On the other hand, anisotropy is observed between the
SLM samples manufactured with vertical and horizontal disposition for this condition,
Crystals 2021, 11, 1196 reaching differences in as-built condition of around 5.3% in the maximum resistance, 17 of 23
18.3% in the yield strength, and 3.3% in the elongation until rupture. The horizontal sam-
ples (Y-axis) were those that presented the highest resistance with the lowest ductility.
Although it is noteworthy
for this condition, that a lowinvariability
this is reflected in the
the reported results was
standard evidenced
deviation of theforresults.
this con-It
dition, this is reflected in the reported standard deviation of the results.
is worth mentioning that heat-treated SLM tensile samples showed a dimpled surface It is worth men-
tioning that indicating
at fracture, heat-treateda SLM tensile samples
transgranular ductileshowed
failure amode
dimpled surface at fracture,
as previously reportedindi-
by
cating a transgranular
Zhang D. et al. [10]. ductile failure mode as previously reported by Zhang D. et al. [10].

Figure 16. Engineering stress–strain curves for SLM samples in different

different conditions.
conditions.

When comparing the mechanical properties obtained between the heat-treated SLM
and investment
investmentcasting
castingsamples,
samples,it itcan canbebe observed
observed thatthat
thetheSLM SLM samples
samples exceedexceed
the me-the
mechanical
chanical resistance
resistance obtained
obtained in the in investment
the investment casting casting
samples samples with standard
with standard heat
heat treat-
treatment,
ment, and adequate
and adequate ductility
ductility is also is also obtained
obtained in allinthe
all conditions
the conditions studied.
studied. Comparing
Comparing the
the best
best results
results obtained
obtained in SLM
in SLM (Y(Y Axis—TT2)
Axis—TT2) withthe
with thebest
bestresults
resultsobtained
obtained forfor investment
investment
casting samples
casting samples(TT0),(TT0),there
thereis ais51.3%
a 51.3%increase in maximum
increase in maximum resistance, with awith
resistance, 66.2%a higher
66.2%
yield
higher yield strength and also a slight increase in the elongation at break of 0.5%.results
strength and also a slight increase in the elongation at break of 0.5%. These These
indicateindicate
results that the expected hardeninghardening
that the expected was achieved wasthrough
achieved thethrough
strengthening mechanisms
the strengthening
Crystals 2021, 11, 1196 by precipitation and dispersion of particles (solid solution),
mechanisms by precipitation and dispersion of particles (solid solution), which18are which are sought ofwith the
24sought
combination of putting into solution and artificial aging in the
with the combination of putting into solution and artificial aging in the standard TT0, standard TT0, taking into
accountinto
taking thataccount
both IN718 alloys
that both IN718havealloys
similar chemical
have similarcomposition in both manufacturing
chemical composition in both man-
routes studied.
conditions and This can
processes be seen
shown graphically
in Figure 17, in the
where comparison
yield
ufacturing routes studied. This can be seen graphically in the comparison strength between
(σy), allbetween
ultimatethetensile
conditions
all the
and processes
strength (UTS),shown
elastic in Figure(E),
modulus 17,andwhere yield strength
the percentage (σy), ultimate
of elongation tensile
at break (ε) are rep-strength
resented.
(UTS), elastic modulus (E), and the percentage of elongation at break (ε) are represented.

Figure
Figure 17. 17. Evolutionofofmechanical
Evolution mechanical properties
properties with
withheat
heattreatments for for
treatments IN718 alloy.
IN718 alloy.

Besides, results reported by other authors for SLMed IN718 samples with similar heat
treatments to those applied in this work are lower. Table 5 shows a comparison of the meas-
ured properties of as built and heat-treated samples with those reported in the literature.

Table 5. Summary of mechanical properties for SLM IN718 alloy in this work compared to other
authors.
 Table
Figure 17. 5. Summary
treatments
Evolution to ofapplied
of those mechanical
mechanical properties
in this
properties work forlower.
are
with heat SLM IN718
Table
treatments alloy
for5 in alloy.
shows
IN718 this work compared
a comparison of thetomeas-
other
authors.
ured properties of as built and heat-treated samples with those reported in the literature.
Besides, results reported by other authors for SLMed IN718 samples with similar heat
+ Homogenization + + Solution +
Figure 17.Table 5. Summary
treatments
Evolution to Mechanical
of thoseofapplied
mechanical mechanicalin this
properties SLM
properties
work
with heatareforlower.
SLM IN718
TableDouble
treatments 5alloy in alloy.
shows this work compared
a comparison + Double
of thetomeas- other
Reference Solution +for IN718 Double
authors.
ured properties of Properties As Built samples with those reported in the literature.
as built and heat-treated Aging
Crystals 2021, 11, 1196 Aging Aging 18 of 23
Besides, results reported by other authors for SLMed IN718 samples with similar heat
σy (MPa) 756.1 ± 2.7 + Homogenization
1243.1 ± 10.6 + +1300.1 Solution± 4.9+ 1420.1 ± 42.3
Figure 17.Table 5. Summary
treatments
Evolution to Mechanical
of thoseofapplied
mechanical mechanicalin this
properties SLM
properties
work
with heatareforlower.
SLM IN718
Table
treatments for5alloy in alloy.
shows
IN718 this work compared
a comparison + Double
of thetomeas- other
Reference
This work UTS (MPa) 1054.5 ± 1.9 Solution 1445.9+±Double 2.7 Double
1508.2 ± 4.2 1567.4 ± 40.5
authors.
ured properties of Properties As Built
as built and heat-treated samples with those reported in the Aging
literature.
Ɛ (%) 30.1 ± 0.2 Aging
18.9 ± 0.4 Aging
17.9 ± 0.5 15.7 ± 0.3
Besides, results reported by other
Besides, authors
results for SLMed
reported by IN718authors
other samplesfor with similar heat
σ
σ (MPa)
yy (MPa) 756.1
590 ± 2.7
± 5 + Homogenization
1243.1- ± 10.6 + +1300.1 Solution
- ± 4.9+ SLMed
1420.1- ±IN718 42.3 samples with similar
Table 5.
treatments Summary Mechanical
of mechanical
to those applied heatin SLM
properties
this work are
treatments for SLM IN718
lower.applied
to those Table 5 shows alloy in this
in this aworkwork
comparison +
compared Double
of theTable
are lower. to other
meas-5 shows a comparison
Reference
This
Li et al.work
[37] UTS (MPa) 1054.5 ±±161.9 Solution
935Built 1445.9-+±Double 2.7 Double
1508.2 - ± 4.2 1567.4 - ± 40.5
authors.
ured properties of Properties
as built of the As
andmeasured
heat-treated samples
properties with
of as those
built reported
and in the
heat-treated Aging
literature.
samples with those reported in
Ɛ (%) 30.1
30 ± 0.2
3 Aging
18.9 -± 0.4 Aging
17.9 -± 0.5 15.7 -± 0.3
σy (MPa) the
(MPa) literature.
756.1 ± 2.7
ofσyymechanical
Table 5. Summary Mechanical 590
849±
SLM
properties 5 for+ SLM Homogenization
1243.1 - ± 10.6
1046
IN718
+ +1300.1
Solution
- ± 4.9
1084
alloy in this work
+ 1420.1- ± 42.3
+ Double
compared to other
Reference
This work UTS (MPa) 1054.5 ±±161.9 Solution + Double Double
Li
Zhang et
Table
authors. al.
et [37]
al.
5.[30] UTS
Summary (MPa)
of
Properties mechanical935
As1126
properties
Built for1445.9 -IN718
1371
SLM ± 2.7 alloy in1508.2
1371
this ± 4.2 compared
- work 1567.4 - ± 40.5
Aging to other authors.
Ɛ (%) 30.1
30 ± 0.2
3 Aging
18.9 -± 0.4 Aging
17.9 -± 0.5 15.7 -± 0.3
22.8 12.3 10.1
σ (MPa)
σyyyy (MPa) 756.1
590 ± 2.7 + Homogenization
1243.1 -- ± 10.6 ++ +1300.1 Solution
- ± 4.9+ 1420.1 -- ± 42.3
σ (MPa)
Mechanical SLM-± 5
849 1046 1084
1185 + Double
Reference
Trosch
This et
work al. Mechanical
UTS (MPa) 1054.5 ± 1.9SLM Solution
1445.9 + Homogenization
Double
± 2.7 Double
1508.2 +
± 4.2 + Solution
1567.4 +
Li et et
Zhang
Reference al.al.
[37][30] UTS (MPa)
Properties
UTS (MPa) 935
As -± 16
1126
Built 1371-- -
1371
1430 -- ± 40.5
Aging + Double Aging
[38] Properties
Ɛ (%) 30.1 ± As Built 18.9
0.2 Aging ± 0.4 Solution17.9
+
Aging± 0.5 Double
15.7 ±Aging
0.3
Ɛ (%)
Ɛ (%) 30
22.8
- 3 12.3-
- Double Aging -
10.1
18.6 -
-
σ (MPa)
σyyyy (MPa) 756.1
590 ± 2.7 1243.1 ± 10.6 1300.1 - ± 4.9 1420.1-- ± 42.3
σ
σ y (MPa)
(MPa) -± 5
849
700 1046
1200 -- 1084
1185
- - 4.9
Trosch
This
Hosseini
Li
Zhang et etal.et
etal.
work
[37]
al. al. UTS
[30]
σy (MPa)
UTS
UTS
(MPa) 1054.5
(MPa)
(MPa) 935
1126
- 161.9 ± 2.7 1445.9
±±756.1 1371 -- ± 2.7 1243.1 ±1508.2
1371
1430
1567.4-±
10.6 - ± 4.2 1300.1
-± 4.2
± 40.5 1420.1 ± 42.3
This work [38] UTS (MPa) 1000 1054.5 ± 1.9 1400 1445.9 ± 2.7 - 1508.2 1567.4 ± 40.5
[2] Ɛ (%) 30.1
30 0.2
-± 330.1 ± 0.2
22.8 18.9
12.3 --± 0.4 17.9 -± 0.5 15.7 -± 0.3
Ɛ (%)
(%) 22 20 18.9 ± 0.4 10.1
18.6
- 17.9 ± - 0.5 15.7 ± 0.3
y (MPa) 590
σ
σ y (MPa)
y
y (MPa) -± 5
849
700 1046
1200
-- -
1084
1185
-
--
-
Trosch
Hosseini
Li et etal.et
etal.
[37]al. UTS σy (MPa) (MPa) 935 590 ± 5 - -- -
Zhang These
Li et al. [37]
al. [30]
results UTS
allow
UTS (MPa)
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(MPa) to confirm -± 16
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--
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-
1371
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- -
[38]
[2] Ɛ (%) 30
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22
3 12.3
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20
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σ
σ y
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700 1046
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σy (MPa) and 849solution) are not completely
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Zhang IN718
et al. alloy
[30]
[38]
[2] obtained
UTS by SLM
(MPa) to improve its
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1371 -
by means of
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[38] results UTS
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by us
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the was concluded
microstructural
IN718 alloy obtained by SLM to improve its mechanical properties, which were obtained in the
analysis microstructural analysis
by means of
in as-built by means
optical microscopy
condition, of optical
andand
due to the fine FESEM microscopy
examination:
homogeneous and FESEM examination:
that microstructure
cellular the first two stages that
with ofsmall first two stages of the
the
standard
and well distributed standard
treatment (homogenization
Laves treatment
and delta and (homogenization
phases solution) are not
at the grain and solution)
completely
boundaries are not completely
thatnecessary
originated inafter
the necessary in the
IN718 alloy obtained by IN718
SLMalloy obtained
to improve itsby SLM to improve
mechanical its mechanical
properties, which were properties,
obtainedwhich were obtained in
as-built
in as-built condition, due to thecondition, due to the fine cellular
fine and homogeneous and homogeneous cellular
microstructure with microstructure
small with small and
well distributed Laves and delta phases at the grain boundaries
and well distributed Laves and delta phases at the grain boundaries that originated after that originated after SLM
processing, which contribute to obtain better mechanical properties including a reasonable
ductility (even higher than that obtained in investment casting with TT0). The influence of
delta phase on the mechanical properties is well known in this alloy [31,39,40]. Improved
mechanical properties were obtained by applying only a stepped direct aging to SLM
samples. This thermal treatment allows, in addition, the refining of delta phase in a needle-
like shape in the interdendritic regions, and the precipitation of γ0 and γ” in the matrix,
improving the mechanical properties obtained in the as-built condition. A similar trend of
improving mechanical resistance with direct double aging of IN718 SLMed samples was
reported recently by Teng Q. et al. [41].
Table 6 shows the summary results obtained in the tensile tests performed on those
samples manufactured by means of investment casting. In all cases, the mechanical
resistance and even the ductility are lower than those obtained with the SLM process with
the same heat treatments.

Table 6. Summary of mechanical properties for IN718 alloy obtained by investment casting.

Investment Casting
Property As-Cast TT0 TT1 TT2
σy (MPa) 434.20 ± 4.05 854.61 ± 42.47 757.76 ± 18.27 769.64 ± 29.95
UTS (MPa) 764.83 ± 39.19 1036.06 ± 25.62 995.79 ± 4.56 1032.78 ± 45.99
E (GPa) 61.78 ± 2.81 167.94 ± 6.00 170.89 ± 2.83 172.96 ± 4.84
ε (%) 28.47 ± 6.87 15.69 ± 3.66 10.02 ± 2.50 15.42 ± 5.37
 Investment Casting
Property As-Cast TT0 TT1 TT2
σy (MPa) 434.20 ± 4.05 854.61 ± 42.47 757.76 ± 18.27 769.64 ± 29.95
UTS (MPa) 764.83 ± 39.19 1036.06 ± 25.62 995.79 ± 4.56 1032.78 ± 45.99
Crystals 2021, 11, 1196 E (GPa) 61.78 ± 2.81 167.94 ± 6.00 170.89 ± 2.83 172.96 ± 4.84
19 of 23
ε (%) 28.47 ± 6.87 15.69 ± 3.66 10.02 ± 2.50 15.42 ± 5.37

Investment casting samples in as-cast state presented low resistance and ductility,
whichInvestment
improved casting samples
significantly in the
with as-cast state presented
application low resistance
of the standard andtreatment,
TT0 heat ductility,
which improved significantly with the application of the standard TT0 heat treatment,
increasing their maximum resistance by 35.5%, their elastic limit by 96.8%, and reducing
increasing their maximum resistance by 35.5%, their elastic limit by 96.8%, and reducing
their elongation at break by 81.5%. As a reference, Figure 18 shows the stress–strain (elon-
their elongation at break by 81.5%. As a reference, Figure 18 shows the stress–strain
gation) of a representative test sample for each condition. Comparing the stress–strain
(elongation) of a representative test sample for each condition. Comparing the stress–strain
curves of both SLM and investment casting samples (Figures 16 and 18 respectively), an
curves of both SLM and investment casting samples (Figures 16 and 18 respectively), an
appreciable difference between the elasto-plastic behavior of the IN718 samples obtained
appreciable difference between the elasto-plastic behavior of the IN718 samples obtained
by both processes can be seen in the as-manufactured state and after the application of
by both processes can be seen in the as-manufactured state and after the application of
different heat treatments.
different heat treatments.

Figure 18. Engineering stress–strain curves for investment casting samples in different
different conditions.
conditions.

Hardness measurements
Hardness measurementswere
werecarried
carriedout
outaccording
accordingtotothe
theUNE-EN
UNE-ENISOISO6507-1
6507-1stand-
stan-
ard to complete the analysis of the mechanical properties. From these measurements, the
dard to complete the analysis of the mechanical properties. From these measurements, the
average and
average and standard
standard deviation
deviation of the measurements
of the measurements were
were calculated,
calculated, which
which are compiled
are compiled
in Table
in Table 7.
7.
Table 7. Hardness values obtained for analyzed conditions.

As-Built/As-
Process/Condition TT0 TT1 TT2
Cast
SLM Y axis 338.8 ± 15.9 504.8 ± 16.8 518.4 ± 13.5 535.1 ± 17.0
SLM Z axis 329.0 ± 5.8 503.4 ± 16.9 508.4 ± 10.3 532.2 ± 17.8
Investment
264.0 ± 47.7 423.8 ± 40.1 408.6 ± 24.2 420.4 ± 28.9
casting

When comparing the values obtained for the different conditions, a similar trend to
that seen in the evaluation of mechanical properties with the tensile tests is observed. The
bar graph in Figure 19 shows the comparison between the IN718 samples obtained by
SLM and the investment casting samples. Comparing samples in the same heat treatment
stage, it can be concluded that in all cases, SLM samples achieve higher hardness values
than investment casting ones. The SLM samples with TT2 present approximately 26.3%
more hardness than the investment casting samples with TT0, which confirms that the
hardening by dispersion of γ0 /γ” particles (solid solution) in the γ nickel matrix allows to
slightly improve the mechanical properties after its SLM processing, applying only stepped
direct aging.
 SLM and the investment casting samples. Comparing samples in the same heat treatment
stage, it can be concluded that in all cases, SLM samples achieve higher hardness values
than investment casting ones. The SLM samples with TT2 present approximately 26.3%
more hardness than the investment casting samples with TT0, which confirms that the
hardening by dispersion of ′/″ particles (solid solution) in the  nickel matrix allows to
Crystals 2021, 11, 1196 20 of 23
slightly improve the mechanical properties after its SLM processing, applying only
stepped direct aging.

Figure 19.
Figure Hardness evolution
19. Engineering for SLM
stress–strain andfor
curves investment casting
investment samples
casting in different
samples conditions.
in different conditions.

Comparing the
Comparing the hardness
hardness values
values obtained
obtained in
in this
this work
work with
with results
results reported
reported by
by other
other
authors, it can be concluded that for similar heat treatments (with small differences in the
authors, it can be concluded that for similar heat treatments (with small differences in the
temperature and times for each stage), higher hardness of the material was achieved with
temperature and times for each stage), higher hardness of the material was achieved with
the process parameters and manufacturing route used. Table 8 shows the comparison of
the process parameters and manufacturing route used. Table 8 shows the comparison of
HRC hardness values reported by other authors and with the results obtained in this work.
HRC hardness values reported by other authors and with the results obtained in this
work.
Table 8. Summary of hardness values (HRC) obtained in this work (mean values converted from HV0.5 measurements on
SLM Y-axis samples) compared to other authors.
Table 8. Summary of hardness values (HRC) obtained in this work (mean values converted from
Condition This HV0.5
work measurements
Zhang eton
al.SLM
[30] Y-axis samples)
Huang compared
et al. [16] to otheretauthors.
Tucho al. [29] Li et al. [37]
As-Built 34 32.5 This Zhang
- et al. Huang et
- al. Tucho et al. 30Li et al.
Condition
+ work [30] [16] [29] [37]
Homogeneization As-Built 34 32.5 - - 30
49 42.5 - - -
+ Solution + + Homogeneization +
Double + Aging 49 42.5 - - -
Solution + Double +Aging
+ Solution + + Solution + Double Aging 50 43 50 45 44
50 43 50 45 44
Double Aging + Double Aging 51 - - - 38
+ Double Aging 51 - - - 38
5. Conclusions
5. Conclusions
After comparing as-built/as-cast and heat-treated microstructures, both manufactur-
ing routes (SLM and investment casting) generate quite different microstructures. The
main conclusions on this aspect are:
• Due to the differences in cooling rates between investment casting and SLM process,
the microstructures generated are completely different. While the one obtained by
investment casting is composed mainly by a dendritic structure, the one obtained
by SLM is characterized by columnar and cellular structures with a very thin cells
microstructure.
• The employment of the homogenization stage in the thermal treatment allows to
achieve the solubilization of undesired phases, which is not the case with the solution stage.
• The double aging treatment at stepped temperatures carried out in the present work
assures the precipitation of γ0 and γ” to improve the mechanical properties obtained
in as-built/as-cast conditions for the IN718 alloy.
After comparing the mechanical properties obtained in both processes, the strength
of SLM samples in as-built and direct-aged conditions exceeds the strength obtained in
investment casting heat treated (TT0), and the ductility measured in SLM samples through
Crystals 2021, 11, 1196 21 of 23

elongation at rupture is satisfactory for both orientations evaluated, since it exceeds the
typical values required for aeronautical parts obtained by investment casting, although
this depends partly on the customer and final application. Related to this, the improved
mechanical properties obtained in the IN718 alloy processed by SLM are mainly affected by:
• The dispersion of γ0 /γ” particles (solid solution) in the γ-Ni matrix and the presence
of a small quantity of delta phases in the interdendritic regions, which allows to
improve the mechanical properties of the material after its SLM processing.
• Due to the fine and relative homogeneous microstructure obtained from SLM process-
ing of IN718 alloy, it is not necessary to apply homogenization and solution stages as in
the standard heat treatment used for this type of alloy obtained by casting or wrought.
The pre-heating and process parameters selected, in combination with direct-stepped
aging heat treatment (at 720 ◦ C/620 ◦ C), provides the material obtained by SLM with
its best mechanical properties.
The SLM process generates a material with adequate strength in as-built condition
compared with the standard heat-treated investment casting IN718 alloy, and the ductility
and hardness are slightly improved with the only application of a direct double-aging
treatment after its manufacture, which does not require the solubilization phase (solution)
commonly used in the standard treatment and widely used in the foundry industry, to
achieve high strength. Apart from the delta phase observed in as-built condition in SLM,
other strengthening mechanisms were found: A combination of solid solutions with fine
precipitation of strengthening phases in the matrix.

Author Contributions: Conceptualization, J.C.P. and P.P.R.; methodology, J.C.P. and J.A.; validation,
J.C.P. and P.P.R.; formal analysis, J.C.P., N.R., J.A., M.C.T.; resources, J.C.P. and P.P.R.; data curation,
J.A. and N.R.; writing—original draft preparation, J.C.P.; writing—review and editing, M.C.T. and
J.C.P.; project administration, J.C.P.; funding acquisition, P.P.R. All authors have read and agreed to
the published version of the manuscript.
Funding: This research was funded by the Basque Government grant KK-2019/00007 (Departamento
de Desarrollo Económico e Infraestructuras del Gobierno Vasco, Programa ELKARTEK Convocatoria
2019) through OPTIFAN project.
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: The data presented in this study are available on request from the cor-
responding author. The data are not publicly available due to confidential non-disclosure agreement.
Acknowledgments: The authors would like to thank the Institute of Materials Technology (ITM)
of the Universitat Politècnica de València (UPV)—Spain and especially Vicente Amigó for the DRX
analysis made.
Conflicts of Interest: The authors declare no conflict of interest.

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