The International Journal of Advanced Manufacturing Technology (2021) 115:3999–4020

https://doi.org/10.1007/s00170-021-07320-y

ORIGINAL ARTICLE

Effect of the parametric optimization and heat-treatment

on the 18Ni-300 maraging steel microstructural properties
manufactured by directed energy deposition
Christian Félix-Martínez 1,2 & Juansethi Ibarra-Medina 2,3 & David Andrés Fernández-Benavides 1,2 &
Luis Alberto Cáceres-Díaz 2,4 & Juan Manuel Alvarado-Orozco 1,2

Received: 9 December 2020 / Accepted: 20 May 2021 / Published online: 12 June 2021
# The Author(s), under exclusive licence to Springer-Verlag London Ltd., part of Springer Nature 2021

Abstract
Maraging steels (MS) are widely used materials for heavy-duty applications and are considered an alternative to carbon hardened
steels when high strength and good toughness is needed. Their processing through additive manufacturing (AM) technologies
offers additional high-value opportunities, for instance, in the rapid prototyping or fabrication of tooling and inserts, and in the
repair of molds and dies as well as in maintenance applications. This work studied the maraging 300 steel (18Ni-300) deposited
by the laser cladding (LC) process. The experimental design was based on a 23-full factorial design used to determine the
optimum processing windows, using a constant powder feed rate. After that, samples with optimal process parameters were
manufactured to determine the influence of deposition strategy and aging heat treatments on structural and mechanical properties
(i.e., macrohardness). Results indicated the influence of crucial process parameters (i.e., laser power, velocity, and laser spot size)
on the track’s geometrical characteristics. The processing windows also revealed that particular combinations of these parame-
ters’ values produced LC tracks with the minimum dilution with either maximum height or maximum width, which is desirable
for manufacturing and repair applications. Although the as-built samples did not show significant differences in their hardness,
they showed a considerable difference in their austenitic phase content due to a combined effect between the sample’s geometry
and deposition pattern. Aging heat treatments between 460 and 490 °C (4–8 h) resulted in the maximum hardness value
(~55HCR) with an austenite content below 6 wt% calculated by Rietveld analysis. Finally, SEM and EDS analysis were carried
out; it was found that the austenite located in the boundaries of the solidification structures is rich in Mo, Ti, and Ni for the
samples in the as-built condition, while for the samples with aging, the highest content of austenite rich in Ni and Mo was
obtained with aging at 530 °C.

Keywords Laser cladding . Maraging steel . Process-structure-properties relationship . Heat treatments process . Additive
manufacturing

1 Introduction

* Juan Manuel Alvarado-Orozco Among additive manufacturing (AM) technologies, laser

juan.alvarado@cidesi.edu.mx cladding (LC) belongs to the directed energy deposition
(DED) processes that have stood out as the most attractive
1
Centro de Ingeniería y Desarrollo Industrial (CIDESI), Av. Playa Pie technique for fabricating, repairing, and coating medium or
de la Cuesta No. 702, Desarrollo San Pablo, Querétaro 76125,
México large tooling/components to yield very high mechanical and
2 metallurgical quality. LC is composed of a deposition nozzle,
CONACYT-Consorcio de Manufactura Aditiva (CONMAD), Av.
Pie de la Cuesta 702, Desarrollo San Pablo, Querétaro, México a high-power laser combined with a feedstock-feeding mech-
3 anism, and a motion system, e.g., a robotic arm or a computer
Dirección de Cátedras-CONACYT, Consejo Nacional de Ciencia y
Tecnología (CONACYT), Av Insurgentes Sur. 1582, numerical control (CNC) system. This AM technology is
CP 03940 México City, México commonly used for processing metallic materials, although
4
Centro de Tecnología Avanzada (CIATEQ A.C.), Eje 126 No.225, it can also be used to process some ceramics or metallic-
Industrial San Luis, 78395 San Luis Potosí, Mexico ceramic composites. Compared with laser powder-bed fusion
4000
(LPBF) technologies, a wider variety of materials can be LC
processed. DED processes permit the use of a high variety of
metals and combination of them and can lead to in situ
alloying. A combination of materials is also possible and can
lead to in situ alloying [1]. Applications of LC are found in
industries such as aeronautics and space, oil and gas, die and
tooling, and mining. Maraging steels (MS) are one of the most
robust metallic materials available for heavy-load applica-
tions, such as high-pressure tooling (injection dies and molds)
and safety-critical aerospace components. The most signifi-
cant aspect involving repair would be choosing an appropriate
filler material; MS are one of those materials and they are
commonly used for the production of plastic injection dies
[2, 3]. These martensitic steels have a low carbon content,
medium amounts of cobalt and molybdenum, large amounts
of nickel, and traces of titanium and aluminum, and combine
high strength, high toughness, good machinability, and
weldability while maintaining a stable performance under me-
chanically demanding environments [4, 5]. These steels have
a very high strength-to-weight ratio. Additionally, the precip-
itation of intermetallic compounds strengthens MS, mainly by
Ni-enriched compounds formed during the aging process [4,
6].
A review of the state-of-the-art shows that AM in MS has
been carried out by mostly using LPBF processes. Most of the
prior research has focused on investigating the microstructure
and mechanical behavior of the processed parts. Suryawanshi
et al. [7] investigated the microstructure and mechanical prop-
erties of maraging 300 steel (18Ni-300) specimens
manufactured by LPBF before and after aging treatments.
Similar mechanical performance to that of conventional
manufacturing was obtained for LPBF 18Ni-300 samples af-
ter aging. Mutua et al. [8] developed a process map for LPBF
with 18Ni-300 material based on laser power, scanning speed,
and energy density. They obtained an improvement in
strength and hardness in specimens after aging treatments
compared to those in the as-built state.
In some cases, the mechanical properties of LPBF parts
were comparable to those of MS in wrought form. Kempen
et al. [9] obtained ultimate tensile strength and yield strength,
greater than the wrought material, in both the as-built and aged
conditions. In the as-built condition, the increase is due to the
natural aging during the SLM process and due to the remelting
of each layer. Tan et al. [10] met the wrought standard require-
ments (ultimate tensile strength and yield strength), while only
the elongation of aging-treated specimens is inferior to the
standard values. They fabricated 18Ni-300 MS by SLM pro-
cess. On the contrary, Meneguetti et al. [11] reported weaker
fatigue properties of samples fabricated by LPBF process than
those produced by vacuum casting. Pardal et al. [12] ex-
plained that low-temperature treatments (T<450 °C) promote
the formation of metastable phases, e.g., S, ω, and Ni3(Ti,
Mo) for long aging times, and at high-temperature treatments
Int J Adv Manuf Technol (2021) 115:3999–4020
(T>450 °C), hardening is produced by the precipitation of
Ni3(Ti, Mo) and then by Fe2Mo phases for the 18Ni-300 al-
loy. De Carvalho et al. [13] reported that precipitation forma-
tion of Ni3X (X=Ti, Mo) occurs during aging, and the forma-
tion of a more stable phase Fe-Mo(Fe2Mo or Fe7Mo6) de-
mands higher exposure times. Casati et al. [14] performed
different aging heat treatments evidencing that reversed aus-
tenite increased after aging, depending on temperature and
time. Moreover, Kempen et al. [9] quantified the phases’ evo-
lution after aging treatments and claimed that as-built parts
were not fully martensitic, presenting austenite under all aging
conditions. This reversion takes place before the re-
dissolution of the Ni3(Ti, Mo) precipitates. Tan et al. [10]
reported that the amount of austenite phase in specimens with
aging treatment increased by comparing with the as-built
specimen, and complete martensite phases are obtained after
solution treatment. Yin et al. [15] also investigated the effect
of aging on the wear rate of LPBF samples. The authors con-
cluded that a solution step, followed by an aging step, was the
preferable heat treatment strategy for 18Ni-300 fabricated by
LPBF, reaching a mechanical response similar to standard
wrought conditions.
Up to now, LPBF processes applied to MS processing have
been comprehensively studied. However, the inherent limita-
tions of powder bed techniques (e.g., small working envelope,
low printing speed, and high capital cost) mean that AM for
MS is still lagging in the development of other high value-
added applications like the fabrication and repair of medium-
and large-sized tools and dies and large structural
components.
Gu et al. [16] mentioned that LC is a suitable DED-AM
technique for addressing the above needs because of its high
deposition rates, in situ alloying capabilities, and better geo-
metrical resolution than “coarse” AM processes like arc-based
AM processes. Despite this, few studies have been published
on LC for MS. For instance, Kürnsteiner et al. [17] reported
the blending of Al particles into a built-in-house MS-like pow-
der (Fe-19Ni) to boost the β-NiAl phase formation strength-
ening the material during LC processing with no heat treat-
ment. Jägle et al. [18] compared the influence of processing
18Ni-300 MS by LC with samples printed by LPBF in terms
of the content of retained and reversed austenite, deposited
nanostructure, density, and chemistry through micro-
hardness measurements. Bergant et al. [19, 20] used LC layers
of 12Ni MS powder to compare three scanning strategies and
observed a cellular microstructure within the track and den-
dritic structure close to the fusion zone. A stable chemical
composition before and after heat treatment was observed in
both the track and substrate; high compressive residual stress-
es were also reported for all scanning strategies. In a separate
study, the same authors [21] compared the influence of 12Ni-
and 23Ni-MS powders deposited on 12Ni-MS substrates by
LC on the mechanical properties of deposits. Clare et al. [22]
Int J Adv Manuf Technol (2021) 115:3999–4020
obtained fully bonded deposited tracks of 18Ni-300 MS on
low-carbon steel by LC and observed a cellular structure in the
tracks with a dendritic structure near the substrate interface.
More recently, Yao et al. [23] deposited 18Ni-300 MS powder
over stainless steel and investigated the influence of the pro-
cessing parameters on tensile strength and hardness.
Previous studies on LC for MS have not focused on devel-
oping processing maps which formalize the effect of process-
ing parameters on the properties of the printed parts. Weng
et al. [24] informed that the optimization of the process pa-
rameters is crucial for the LC technique, in order to achieve
reproducible geometrical characteristics, such as height,
width, and dilution levels. Control over these characteristics
is fundamental for developing any LC process specification
using MS for industrial applications. A key challenge to re-
ducing dilution levels and balance the height-to-width ratio is
to properly establish an operational map (or window) of the
processing parameters (e.g., laser power, powder feed rate,
scanning velocity, and laser spot size) that ensures the LC
deposition of tracks, layers, and walls with the desired geom-
etry and mechanical properties. Leong et al. [25] provided a
basis for such processing parameter windows in terms of laser
beam irradiance. They estimated thresholds for inducing sur-
face melting or welding for various materials. This can be
applied to define irradiance limits on LC processes, where
processing parameters must ensure a shallow substrate melt-
ing without reaching the onset of keyhole formation. Lin [26]
focused on the quality characteristics of dilution rate and ob-
tained that the single most important consideration with regard
to the effects on the dilution rate of laser cladding process is
laser power. Sun and Hao [27] developed a mathematical
model to predict the geometry of cladding coatings within
the relative error of 7%. They found that powder feed rate is
the most significant factor in the ratio width to height, layer
width, and layer height, while laser scanning speed has the
strongest effect on the molten pool and increasing laser power
can increase layer width. Angelastro et al. [28] proposed an
analytical methodology for optimizing LC processing of
Colmonoy 227-F. They analyzed key process parameters (la-
ser power, powder feed rate, spot size, overlap) to optimize
process velocity and track geometry. In order to establish pro-
cessing maps, an understanding of the individual and com-
bined effect of the critical process parameters is required.
Some studies have reported the use of statistical techniques
for establishing LC processing maps for materials other than
MS. Graf et al. [29] analyzed LC in MRO applications using a
full factorial design, and Mahamood [30] optimized the LC’s
efficiency using a titanium alloy through a two-level factorial
design. Taguchi methodologies have been applied to the op-
timization of LC for various cases and materials, including
ZE41A-T5 magnesium alloy, cobalt alloy, and Ni-Cr-B-Si
metallic-matrix tungsten carbide (WC), and in turbine repair
applications. Cao et al. [31] applied Taguchi experimental
4001
design to obtain a process window for minimal dilution ratio
by optimizing process parameters. Dubourg and St-Georges
[32] used a combination of Taguchi and EM methods to de-
sign the experiments to obtain the influence of different laser
cladding parameters on the clad geometry and the WC content
for single pass and multipass cladding. Lee [33] studied the
effects of the cladding parameters on the deposition efficiency
by Taguchi method. Lin [26] applied Taguchi method to de-
termine the optimal parameters for tenon repair on a steam
turbine blade using multi-layer laser cladding. Finally, central
composite design (CCD) and response surface methodology
(RSM) have also been applied to LC using Ti6Al4V [27].
This paper investigates the LC process using 18Ni-300 MS
powder deposited on the same material at a constant powder
feed rate of 14 g/min. The separate and combined effects of
three process parameters are presented and discussed to reveal
the relation between the process, structure, and properties of
the built samples. The effect of different aging heat treatments
on the hardness and the austenitic content is presented and
discussed. This work is significant as it develops a map of
LC process behavior using 18Ni-300 and its performance,
which can be directly used to establish LC process specifica-
tions for high-value applications.
2 Materials and experimental procedure
2.1 Materials
Commercially available 18Ni-300 powder (Carpenter, USA)
was used in this study. Figure 1 shows the morphological and
size characteristics obtained using a Jeol JSM/6610LV scan-
ning electron microscope (SEM) and a Sympatec Helos laser
diffraction particle analyzer, respectively. The gas-atomized
powder comprised particles with a regular spherical shape
and only small adhered satellites. The particle size distribution
narrowed to a range with a D10 = 51.7 μm, D50 = 83.84 μm,
and D90 = 129.8 μm, which was adequate for the LC hardware
used. The chemical composition of the powder, measured
using energy-dispersive X-ray analysis (EDX) within the
SEM microscope, is shown in Table 1. The substrate material,
which consisted of round plates (25.4 mm in diameter, 5 mm
in thickness), was cut from an 18Ni-300 rod (Magellan
Materials, USA). This material was chosen due to its avail-
ability and close similarity in chemical composition (see
Table 1) to the powder material, which was relevant to avoid
alloying effects during its melting and heat transfer that could
have occurred if a different substrate material had been used.
Hence, this ensured that the study focused solely on the effect
of the process parameters on the printed sample features.
Figure 2 shows the microstructure of the 18Ni-300 sub-
strate, observed using an Epiphot 200 Nikon optical micro-
scope. Metallographic preparation was conducted by grinding
4002 Int J Adv Manuf Technol (2021) 115:3999–4020

Table 1 Chemical composition of materials used randomized combinations of the selected factors and levels:
Chemical composition (wt%) laser power (800 W and 1200 W), velocity (5 mm/s and 10
mm/s), and laser spot size (2.55 mm and 2.86 mm). The re-
Ni Co Mo Ti Fe sponses analyzed were the dilution and porosity levels and
track height, width, and depth. Figure 3 shows the experimen-
Substrate Nominal* 18.54 9.29 4.84 0.63 Bal.
tal setup used. The substrates were placed on a flat fixture and
Measured** 19.15 10.86 4.93 0.89 Bal.
clamped using a lateral three-point fixture device. The robotic
Powder Nominal* 17.9 9.1 5.0 0.8 Bal.
arm provided the motion and velocity of the deposition head.
Measured** 18.50 9.70 4.90 1.00 Bal.
The tracks were deposited according to a defined linear
Track a Measured** 18.77 9.88 4.84 0.79 Bal.
motion spanning the diameter of the round substrates. The
*Manufacturer spec sheet nozzle’s standoff distance was kept constant at 16 mm, and
**Energy-dispersive X-ray spectroscopy (EDS) velocity was kept constant along a single deposition track but
a
Corresponding to run 2 from Table 3
varied across experiments. The powder feeder provided the
powder stream mass flow rate at a constant level of 14 g/min
to obtain minimum dilutions with maximum height or maxi-
and cloth-polishing, using up to 1 μm of alumina. Then, a mum width. Argon gas was used as the auxiliary gas both for
chemical etching was done on a polished surface using a mod- carrying particles and for providing an inert atmosphere to
ified fry’s solution (50 ml HCl, 25 ml HNO3, 1 g CuCl2, minimize oxidation. The carrier and shielding gas flows were
150 ml H2O) with immersion times of 5 s. The observed kept fixed at 12 l/min. The laser was operated in continuous-
microstructure was typical of the 18Ni-300 alloy, with mar- wave (CW) mode, and the power was kept constant along a
tensite and austenite visible regions, with martensite grains single deposition track. The laser spot size was modified by
homogeneously distributed over the sample surface. defocusing via adjustments to the collimating lens of the de-
position head. The spot size was varied across experiments,
2.2 Experimental setup according to Table 3.
Before deposition, the substrates were cut to thickness
LC deposits were carried out using an LC robotic cell installed using a Pilous TMJ bandsaw cutter and de-greased using eth-
at the Consortium for Additive Manufacturing (CONMAD, anol. After deposition, the tracks were cut in the transverse
CIDESI) in Mexico, which comprises a Trumpf TruDisk 6002 direction in the middle, the most stable zone in a track, as
laser source, an ABB IRB6620-120 robotic arm, a twin- shown in Fig. 4a. This preparation ensured that the unstable
hopper Medicoat flowmotion duo vibration powder feeder, beginning and the end-of-tracks were not considered in the
and a Trumpf BEO D70 three-port coaxial laser deposition analyses. The metallographic sample was prepared as follows:
head. The characteristics of the equipment are summarized after cutting, the samples were mounted in resin and ground
in Table 2. using 180-to-1200-grit SiC paper, followed by polishing
The design-of-experiments (DoE) methodology was used using 1-μm alumina particles. Two etching procedures were
to analyze the influence of the process parameters and deter- applied. First, the samples were etched in 20% Nital (80 ml
mine an optimum processing window for 18Ni-300 deposi- ethanol, 20 ml HNO 3 ) for 5 s in order to analyze its
tion using a constant powder feed rate of 14 g/min. The design mesostructure. After that, the samples were etched in modified
was a 23-full factorial design (three factors with two levels fry (50 ml HCl, 25 ml HNO3, 1 g CuCl2, 150 ml H2O) for 5 s
each) with two replicates. The treatments were obtained from to reveal the microstructure.

Fig. 1 a SEM micrograph of MS

powder particles, b measured
particle size distribution plot for
MS powder
Int J Adv Manuf Technol (2021) 115:3999–4020 4003

Fig. 2 Optical microscope images of the 18Ni-300 MS substrate microstructure

Figure 4b shows the cross-section of a representative Nital-
etched track, where the fusion and heat-affected zones can be
observed. Samples were analyzed using an Epiphot 200
Nikon optical microscope. Figure 4c shows the analyzed geo-
metrical features as follows: track width (W), track height (h1)
as measured from the substrate’s top surface represented by a
dotted line, track depth (h2) as measured below the dotted line,
and the top and bottom track areas measured above and below
the line, respectively. Dilution was calculated according to the
following relation:
A2
Dð%Þ ¼  100
A1 þ A2
where D is the dilution in percent values, A1 is the area corre-
sponding to the top of the track, and A2 is the area correspond-
ing to its bottom.
Porosity was measured by imaging techniques using the
ImageJ software. The analysis was done using micrographs
of the cross-section of the track, as shown in Fig. 4d. The
entire area of the track was first measured, followed by mea-
suring the area of individual pores. Porosity levels were deter-
mined as the ratio of the sum of areas of the individual pores to
the total area of the track.
ð1Þ
2.3 Statistical analysis

Experimental responses were processed using the Minitab®

Table 2 Specifications of robotic LC cell statistical software by analyzing the system variance
(ANOVA) at a significance level of 0.05 (i.e., a confidence
Characteristic Condition Units
level of 95%). The individual influence of the selected factors
Laser operation modes CW/pulsed – and the trend to optimize the studied responses were identified
Wavelength 1030 nm through contour plots. The combined effects of the factors and
Maximum laser power 4000 W responses were analyzed by following the simultaneous opti-
Process fiber core diameter 200 μm mization of several responses. Finally, a suitable combination
Minimum laser spot size 400 μm of processing parameters of LC that can produce either high or
Maximum linear scanning velocity 1600 mm/s wide tracks was identified by calculating the global optimum
in the feasible regions obtained simultaneously.
4004 Int J Adv Manuf Technol (2021) 115:3999–4020

Fig. 3 Experimental setup: a

overall scheme and b close-up
view of the clamped substrate
showing a deposited track

2.4 Structural and hardness characterization
Once the optimal processing parameters were established in
Section 2.3, four rectangular built-ups with a 6 × 30 ×
110 mm (H × W × L) size were manufactured with six depos-
ited layers per sample at the following energy densities: 55.94
J/mm2 (samples A and B) and 36.90 J/mm2 (samples C and D).
Samples were fabricated using a bidirectional deposition pat-
tern with two different stacking strategies between layers: (i)
without rotation between layers (samples A and C) and (ii) with
90° rotation between adjacent layers (samples B and D).
Table 4 summarizes the processing parameters which were ap-
plied for manufacturing the rectangular samples. After deposi-
tion, pieces of 5 mm in thickness were sliced in the middle of
each sample using a disk cutter for their subsequent analysis.
MS are commonly subjected to a two-stage thermal treatment
aiming to achieve their high strength level [13], solution heat
treatment followed by aging heat treatment. According to the
literature, solution heat treatment can vary between 815 and
825 °C [8, 34, 35], and aging treatments between 455 and 510

Table 3 Experimental design and results of responses

Sample Process parameters Response values Combined parameter

Laser power Velocity (mm/s) Spot size Dilution Height Width Depth Porosity Energy density
(W) (mm) (%) (mm) (mm) (mm) (%) (J/mm2)

1 800 5 2.55 8.01 1.24 2.53 0.13 0.62 62.75

2 1200 5 2.55 31.91 1.26 2.93 0.90 0.56 94.12
3 800 10 2.55 11.42 0.58 1.87 0.07 1.39 31.37
4 1200 10 2.55 30.35 0.72 2.47 0.48 0.99 47.06
5 800 5 2.86 2.71 1.34 2.63 0.05 0.81 55.94
6 1200 5 2.86 8.00 1.37 3.18 0.10 0.74 83.92
7 800 10 2.86 8.10 0.61 1.86 0.08 1.67 27.97
8 1200 10 2.86 14.39 0.67 2.5 0.10 0.95 41.96
9 800 5 2.55 6.95 1.23 2.38 0.13 0.51 62.75
10 1200 5 2.55 31.50 1.27 2.85 0.88 0.47 94.12
11 800 10 2.55 9.15 0.57 1.78 0.06 1.23 31.37
12 1200 10 2.55 29.12 0.72 2.46 0.48 0.81 47.06
13 800 5 2.86 2.10 1.39 2.59 0.06 0.67 55.94
14 1200 5 2.86 7.89 1.37 3.19 0.12 0.57 83.92
15 800 10 2.86 7.12 0.6 1.49 0.08 1.36 27.97
16 1200 10 2.86 13.53 0.68 2.53 0.10 0.83 41.96
Int J Adv Manuf Technol (2021) 115:3999–4020 4005

Fig. 4 a Top view of deposited

track spanning across the
substrate length. b Transverse
cross-section of a typical deposit-
ed track. c Illustration of mea-
sured geometrical characteristics,
where W stands for track width,
h1 is track height, and h2 is track
penetration. d Representation of
area of pores

°C [10, 36]. Heat treatments were carried out in a Briteg TH1400
tube furnace. All samples were solution treated at 820 °C for 1 h.
Moreover, different aging temperatures were done in the range of
460–530 °C, varying the treatment duration from 1 to 8 h. All
heat treatments were done under an air atmosphere.
The structural characterization of as-built and heat-treated
samples was carried out using a Rigaku SmartLab
Diffractometer with Cu tube (λ = 1.54056 Å). X-ray diffrac-
tion (XRD) patterns were measured over a 2θ range from 30°
to 120° using the parallel beam mode. For the samples in as-
built condition, three measurements were made along the sam-
ples’ thickness (i.e., bottom, middle, and top) in order to eval-
uate the effect of processing parameters in the austenite vari-
ation. A Rietveld Refinement analysis of the XRD patterns
was subsequently performed using GSAS® to quantify the
austenite and martensite phase fraction of samples. Finally,
the hardness profiles were measured in a Wilson Tukon
1202 micro indenter using a load of 300 gf during 11 s, ac-
cording ASTM E384 [37].
3 Results and discussion
Laser power, velocity, and laser spot size were the factors
chosen for this study based on our previous experience with
this material. Moreover, these factors have been previously
reported in the LC process literature using materials other than
MS; e.g., Lin [26] reported the laser power, powder feed rate,

Table 4 Processing parameters to manufacture the rectangular samples and deposition time per layer

Sample Layer Deposition time Idle time per Total time Total building Energy density (J/mm2)
per layer (s) layer (s) per layer (s) time (s)

P= 800 W 1 to 6 396 10 406 2436 55.94

v= 5 mm/s
Sample A (NR)
P= 800 W 1, 3, 5 396 10 406 1218 55.94
v= 5 mm/s 2, 4, 6 396 46 442 1326
Sample B (R)
P= 950 W 1 to 6 240 17 257 1542 36.96
v= 9 mm/s
Sample C (NR)
P= 950 W 1, 3, 5 240 17 257 771 36.96
v= 9 mm/s 2, 4, 6 204 57 261 783
Sample D (R)
4006
and scan rate (velocity); Sun and Hao [27] the laser pow-
er, scanning speed (velocity), and powder feed rate; and
for MS, Yao et al. [23] the laser power, scanning speed
(velocity), and powder feed rate. The powder feed rate
was set to 14 g/min, which was the most stable rate
with the powder feeder used by previous group obser-
vations. The feed rate was kept constant during all de-
positions. The levels of the factors were chosen through
a preliminary round of experiments carried out before
this study, where laser power ranging from 800 to
1200 W, at a velocity from 5 to 10 mm/s, and spot
size from 2.55 to 2.86 mm produced stable tracks with
a homogeneous geometry. Figure 5 summarizes the de-
posited tracks in a cross-sectional view, corresponding
to the experimental design’s first replicate from sample
number 1 to 8 of Table 3. The rows correspond to the
two spot sizes and the columns to the two velocities
used. Laser power was compared in pairs within each
cell of the table. All tracks showed full metallurgical
bonding with the substrate and a homogeneously distrib-
uted porosity inside the tracks. Porosity was found to be
between 0.47 and 1.7% for all tracks. It is also evident
that the maximum depth of penetration corresponds to
the track deposited at the maximum laser power and
minimum spot size for each velocity setting. Overall,
the tracks made with a velocity of 5 mm/s showed a
much more substantial build-up in volume.
Figures 6 and 7 show the track microstructure for low (be-
low 3%—sample 5) and high dilutions (above 30%—sample
2), respectively. The insets show details of the track core (zone
a), the substrate–track interface (zone b), and the heat-affected
zone (HAZ) (zone c). In both figures, both the austenite in a
martensitic matrix are visible after LC.
Grain orientation within the track is columnar at the core
and changed to equiaxed as it approaches the top, which is
inherent to LC process condition. Regardless of the process
parameters, the austenitic- and martensitic-rich regions were
visible at the track–substrate interface and track external–
surface interface, respectively. At the interface of the substrate
and HAZ, slight grain growth was observed. In the case of
very low dilution, the martensite grains appeared finer than
those in the high-dilution condition. The latter occurs because
a higher-energy input reduced the cooling rates and allowed
for a longer time for grain growth.
1Furthermore, Table 1 shows the chemical composi-
tion of the track after LC, where no significant changes
were observed for both the powder and the substrate,
which further shows that the deposit persisted as 18Ni-
300 material, which is desirable. Table 3 shows the
applied 23-full factorial design, where the randomized
experimental treatments with their corresponding param-
eters are listed in the columns corresponding to the
header process parameters. The response values of
Int J Adv Manuf Technol (2021) 115:3999–4020
dilution, height, width, depth, and porosity were mea-
sured and calculated as described in Section 2. They are
shown in columns corresponding to the header
“Response Values.” Table 5 shows the final ANOVA,
which shows that factors (process parameters) were sta-
tistically significant for all analyzed responses. Laser
power was the most significant factor influencing dilu-
tion, and, in the case of height, width, depth, and po-
rosity, velocity was the most significant factor. It is
worth noting that the studied factors and their effects
explain over 89% of the variation in responses, as evi-
denced by the correlation coefficients (R2adj) from the
ANOVA. The statistical regression models of Eqs. 2–6
correspond to a mathematical prediction of responses:
Dilution ð%Þ ¼ −391:2 þ 0:5717*P þ 16:91*V ð2Þ
þ 132:5*Ø−0:02537*P*V−0:1958*P*Ø−5:66*V*Ø
þ 0:00901*P*V*Ø
Height ðmmÞ ¼ −1:052 þ 0:000909*P þ 0:0401*V ð3Þ
þ 1:185*Ø þ 0:000045*P*V−0:000403*P*Ø
−0:08065*V*Ø
Width ðmmÞ ¼ −1:59 þ 0:000675*P þ 0:229*V
þ 1:613*Ø
þ 0:000117*P*V−0:1774*V*Ø ð4Þ
Depth ðmmÞ ¼ −17:141 þ 0:023452*P þ 0:9728*V ð5Þ
þ 5:931*Ø−0:001425*P*V−0:008113*P*Ø
−0:3323*V*Ø þ 0:000491*P*V*Ø
Porosity ð%Þ ¼ −1:976 þ 0:000947*P þ 0:3311*V
þ 0:411*Ø−0:000224*P*V ð6Þ
where P is laser power, V is velocity, and Ø is the laser
spot size. Further statistical analysis was used to analyze
the process behavior and optimize the process parame-
ters. Figure 8 shows the trends of process behavior at a
spot size of 2.86 mm. Each stripe in the contour plots
indicates a range of values describing the process be-
havior under specific combinations of factors within the
experimental region. These contour plots describe trends
to separately optimize track dilution, height, depth,
width, and porosity. The effect and trend to minimize
dilution and depth levels are shown in Fig. 8a and d,
respectively. The minimum values of dilution and depth
were reached at the lower laser power and velocity
levels, respectively. Figure 8b and c show that the max-
imum track height and width were reached at upper
levels of power and lower velocity levels, respectively.
Finally, Fig. 8e shows that the minimum porosity was
attained at higher laser power and lower velocity levels.
Int J Adv Manuf Technol (2021) 115:3999–4020 4007

Fig. 5 Macrographs of deposited tracks in cross-sectional view. Numbering corresponds to run number in Table 3

Fig. 6 Macrograph of deposited track (sample 5 from Table 3) showing low dilution. Power = 800 W, velocity = 5 mm/s, spot size = 2.86 mm
4008 Int J Adv Manuf Technol (2021) 115:3999–4020

Fig. 7 Macrograph of deposited track (sample 2 from Table 3) showing higher dilution. Power = 1200 W, velocity = 5 mm/s, spot size = 2.55 mm

These trends can be used to determine the process pa-
rameter settings, which can be used to generate shallow
and wide tracks, on the one hand, suitable for coating
applications and high tracks on the other, suitable for
vertical build-ups.
The behavior observed in the contour plots can be under-
stood by analyzing the influence that the individual and com-
bined process parameters have on the output, particularly the
dilution. As discussed, increasing laser power led to increases
in track width, height, and depth, but more markedly in dilu-
tion. For instance, in sample 2, a more than 30% increase in
dilution was observed, as shown in Fig. 7. According to
Pinkerton and Li [38], the melt pool’s temperature increased
with laser power, allowing for deeper material penetration,
which in turn drove higher dilution [39]. Moreover, widening
the laser spot size led to a reduction in dilution when an

Table 5 Analysis of variance (ANOVA)

Dilution (%) Width (mm) Height (mm) Depth (mm) Porosity (%)

Effects F P-value F P-value F P-value F P-value F P-value

Laser power (LP) 1238.43 0 131.25 0 66.18 0.000 327.7 0.000 26.18 0.000
Velocity (V) 58.21 0 149.78 0 7491.81 0.000 15087.42 0.000 87.63 0.000
Spot size (SS) 896.61 0 2.59 0.138 51.25 0.000 35.71 0.000 4.95 0.048
Laser power × velocity 6.28 0.037 5.54 0.024 34.31 0.000 258.31 0.000 15.29 0.002
Laser power × spot size 405.17 0 – – 10.59 0.010 43.79 0.000 – –
Velocity × spot size 43.28 0 4.68 0.056 66.18 0.000 47.41 0.000 – –
Laser power × velocity × spot size 12.52 0.008 – – – – 26.36 0.001 – –
R2adj 99.44% 95.08% 99.81% 99.92% 89.66%
Int J Adv Manuf Technol (2021) 115:3999–4020
increase in laser spot size enlarged the irradiated area, causing
a reduction in power density and giving a more homogeneous
of it over the irradiated area [30].
Moreover, the Gaussian-like energy distribution typical of
a disk laser beam was observed as the drop-in distribution
crest when defocused [40]. As it is well known in laser fusion
processes, a smaller overall power density and lower peak
value on the beam energy distribution directly lead to lower
penetration due to a lower peak temperature in the melt pool
being reached [41], hence reducing dilution.
For its part, changing velocity can yield two effects:
a. Increasing velocity can lead to decreasing dilution. As
already noted, dilution is directly related to the depth of
melt penetration and, according to Powell et al. [39], de-
creasing melt pool depth when the higher velocity was
applied is a result of the interaction time effect; i.e., the
beam irradiates for a shorter time a given unit area, caus-
ing less energy being imparted to the substrate.
b. Under certain process conditions, decreasing velocity can
decrease dilution, which runs counter to the interaction
time effect alone. Under these circumstances, lower dilu-
tion occurs with increasing interaction time caused by a
lower velocity, increasing the melt pool size. As shown by
Fathi et al. [42], this increases track width and height, and
reduces energy reaching the substrate, thus inhibiting
dilution.
This later behavior can be observed in Fig. 9a, which
shows the dilution in terms of the energy-density param-
eter, defined as in Table 3. Two clearly defined main
groups can be observed (highlighted by the grey ellipse
shapes) in this figure, corresponding to the velocity levels.
Generally, lower dilution can be observed in the higher-
energy-density group at a velocity of 5 mm/s compared to
the lower-energy-density group at a velocity of 10 mm/s.
Furthermore, arrows indicate pairing sub-groups where
laser power and spot size are equal in both, but that ve-
locity decreases. Sub-groups 1 and 2 correspond to a low
laser power setting, and sub-groups 3 and 4 correspond to
a high laser power setting. The arrows’ direction indicates
that the track grows in size from one side of the group to
the other with decreasing velocity, as shown in Fig. 9c for
sub-group 2 and Fig. 9d for sub-group 3. In most cases, it
is clear that reducing the velocity led to track growth and
an associated decrease in dilution.
Overall, dilution levels below 15% were observed for three
of the four sub-groups. Moreover, an observation of the main
groups (grey ellipses) shows the effect of reducing the spot
size on dilution. For instance, when considering the low laser
power setting, decreasing the spot size slightly increased dilu-
tion. However, decreasing spot size produced a significant
dilution increase despite the relatively small increase in energy
4009
density when considering the high laser power setting. These
observations suggest that at laser power levels above a thresh-
old (presumably below but close to 1200 W), slightly decreas-
ing spot size can cause a significant increase in dilution, which
is thought to occur because reducing the laser spot size re-
duces the irradiated area, along with a higher peak value of
the crest of the Gaussian-like energy distribution. These ef-
fects could have led to much higher penetration, which, in
turn, would have increased dilution levels.
Figure 9b shows the behavior of track height, width, depth,
and porosity in terms of energy density. Porosity tended to
decrease at higher energy densities, which suggests that higher
melt pool temperatures allow for better conditions for the
formed bubbles within the pool to escape. Note that the po-
rosity decrease was not linear, although a plateau was expect-
ed at higher energy levels. A clear trend was observed for
track dimensions (i.e., height, width, and depth), where incre-
ments in the energy density led to gradual growth in track
dimensions. This increase was more pronounced in the height
and width but was less marked in the case of track depth. As it
has been discussed, this implies that when a track grows more
extensive due to higher energy density, growth above the sub-
strate’s surface was dominant compared with growth below
the surface, and thus dilution did not grow at higher energy
densities.
Figure 10 presents the overlaid contour plots showing re-
gions where the combination of process parameters is such
that tracks can be produced with maximum width in one case
and maximum height in the other. The latter is maintained
while maintaining minimum dilution and depth. These feasi-
ble white regions are known as the local optima. The region to
obtain 18Ni-300 MS tracks with the maximum width and
minimum remaining responses was optimized in the follow-
ing narrow ranges (Fig. 10a): porosity (0.8–1.2%), dilution
(5–10%), height (0.8–0.9 mm), width (2.0–2.6 mm), and
depth (0.02–0.09 mm). The optimum combination of process
parameters to predict the maximum track width was as fol-
lows: laser power, 949.3 W; spot size, 2.86 mm, and velocity,
8.8 mm/s. Similarly, the region to obtain tracks with the max-
imum height and minimum values of the remaining responses
was optimized in the following narrow ranges (Fig. 10b): po-
rosity (0.7–0.86%), dilution (0.05–8%), height (1–1.4 mm),
width (2.5–2.7 mm), and depth (0.01–0.07 mm). Therefore,
the optimized combination of process parameters to deposit
tracks with the maximum height is as follows: laser power at
800.9 W, spot size at 2.86 mm, and velocity at 5 mm/s.
These optimal local predictions represent a powerful tool
that can be readily used to determine LC’s process specifica-
tions using 18Ni-300 MS. For instance, coating applications
where a wider track would be desired or 3D build-up applica-
tions, where a high track is favored. Both cases of optimum
predictions of parameters: (i) a wide-and-shallow deposit and
(ii) a high deposit were experimentally validated. Figure 11
4010 Int J Adv Manuf Technol (2021) 115:3999–4020

Fig. 8 Contour plots of 18Ni-300 MS deposited tracks for a dilution, b height, c width, and d depth

shows the runs of experimental validations carried out using
the process parameters specified in Fig. 10. For case (i), a
shallow track 0.71 mm high was produced (see Fig. 11(a)),
similar to the predicted value (0.81 mm). A corresponding
layer was also deposited, and a visual inspection revealed
acceptable characteristics (see Fig. 11(b)). For case (ii), a high
track 1.31 mm in height was deposited (see Fig. 11(c)), in
good agreement with the predicted values (1.37 mm). A ver-
tical five-layer build-up was also manufactured and is shown
in Fig. 11(d). Proper bonding was observed between layers

Fig. 9 a Effect of energy density on dilution, b effect of energy density on track characteristics, c effect of velocity on sub-group 2, and d effect of
velocity on sub-group 3
Int J Adv Manuf Technol (2021) 115:3999–4020
with a slight wall tilting. In both cases, the dilution levels were
above the predicted values, but the agreement achieved with
the other track characteristics supports the usefulness of the
optimized parameters and the statistical model.
The austenitic phase evaluation and the mechanical char-
acterization (i.e., macrohardness) were carried out in samples
A to D in the as-built conditions and after heat treatments.
Results are summarized in Fig. 12(a). On the one hand, sam-
ples A and C were manufactured by following the cladding
pattern between layers shown in Fig. 12(b). On the other hand,
samples B and D were manufactured rotating 90° the cladding
direction between layers in Fig. 12(c). XRD patterns of sam-
ples A–D in as-built conditions are shown in Fig. 13(a), where
the presence of the austenite peaks γ (111), γ (200), and γ
(220) can be observed. Figure 13(b) shows variation in the
peak intensities for the γ (111) plane, which shows differences
in the austenite amount between samples. On the other hand,
Fig. 13(c, d) shows the XRD patterns for samples A–D after
an aging treatment at 480 °C for 6 h, showing a decrease in the
austenite compared to the as-built condition. In order to quan-
tify the austenite phase in all tested samples, a Rietveld anal-
ysis of XRD spectra was carried out using the General
Structure Analysis System (GSAS) software [43]. Results
are plotted in the second y-axis of Fig. 12(a). The austenite
content in the as-built samples was as follows: sample A
(27.51 ± 3.45 wt%), sample B (23.68 ± 2.70 wt%), sample
C (16.07 ± 1.95 wt%), and sample D (10.66 ± 3.07 wt%). The
austenite variation in the as-built samples is due to a combined
effect of the sample’s rectangular geometry (see Fig. 12(b, c))
and the processing variables (see Table 4), including the ve-
locity and the increase in the idle time between rotated and
non-rotated samples.
The hardness behavior evidenced a negligible variation in
the as-built samples, independently of the stacking strategy
between layers and different energy densities, i.e., 55.94
J/mm2 (samples A and B), and 36.90 J/mm2 (samples C and
Fig. 10 Overlaid contour plots to simultaneously optimize a width and b height. The white zone represents a feasible region where a suitable
combination of process parameters is identified
4011
D). Although the LC process has a cooling rate of ~104 °C/s
[18], the obtained hardness values of 33.71 ± 1.01 HRC (at
55.94 J/mm2) and 34.11 ± 1.18 HRC (at 36.90 J/mm2) were
very similar to those reported by the LPBF process (32–36
HRC) with higher cooling rates up to ~108 °C/s. Campanelli
et al. [44] reported a maximum value of hardness of 34 HRC
for the scan speed and laser power set respectively to the
minimum and the maximum value of the considered range;
Jägle et al. [18] obtained ~32 HRC and Tan et al. [10] obtained
a maximum value of hardness of 36 HRC within optimized
parameters.
Figure 14 compares the as-built microstructure correspond-
ing to samples A (Fig. 14a–d) and D (Fig. 14e–h) at different
magnifications. In both conditions, the austenite phase is lo-
cated at the interdendritic boundaries of the solidified struc-
tures promoted by the elemental segregation differences,
which agrees with other literature reports. For instance, Yin
et al. [15], Conde et al. [45], and T. Allam et al. [46] reported
in samples in the as-built condition that the presence of
retained austenite is related to strong local compositional seg-
regations at the cellular/dendritic boundaries during solidifi-
cation. Besides, Casati et al. [14] showed that the austenitic
phase is mainly located at the boundaries with the martensite
blocks. Figure 15 correlates specific microstructural images
with the EDS elemental mapping for samples A and D in as-
built conditions. For sample A (Fig. 15a), the austenite area at
the boundaries of the solidification structures looks larger than
the austenite area corresponding to sample D (see Fig. 15b).
Local EDS measurements showed that austenite is richer in
Mo (7.0%), Ti (1.5%), and Ni (18.8%) compared to Mo (5.0),
Ti (1.0%), and Ni (18.5%) measured in the powder measured
in weight percent. From the above, it can be said that austenite
is enriched in Mo and Ti as confirmed by the EDS mapping.
On the contrary, in the martensite phase (matrix), less Ni
(17.4%), Mo (4.3%), and Ti (0.3%) were observed compared
to the feedstock powder, in sample D, similar results with
4012
Fig. 11 LC formed using optimized parameters for coating and vertically built-up applications, showing (a, c) single-track and (b, d) multiple-track
deposits
marked Mo (6.7%) and Ti (1%), Ni (18.8%) enrichment in the
austenitic phase (see Fig. 15b). Both samples (A and D)
showed the presence of cubic precipitates rich in N and O,
suggesting the presence of nitride result of the interaction with
surrounded deposition atmosphere. This result agrees with
Thijs et al. [47], who reported the presence of TiN inclusions
for an SLM process in N-rich atmospheres.
After solution+aging heat treatments, the macrohardness
significantly increased to about 54 ± 2 HRC. The hardness
enhancement occurs because of the Ni, Mo, and Ti in solution
separates from the matrix and forms Ni3Mo, Fe2Mo, and
Ni3Ti compounds, leading to a strengthening of hardness by
precipitation [48]. Figure 16 compares specific microstructur-
al images with the EDS elemental mapping for sample A at
two different heat treatments: aged at 480 °C for 6 h (Fig. 16a)
and aged at 530 °C for 1 h (Fig. 16b). The austenite content
with blocky-like morphology [45] is greater and more evident
in the sample treated at 530 °C and 1 h. This increase could be
related to the dissolution of the intermetallic compounds Ni3Ti
and Ni3Mo as reported by [9, 14, 49]. The austenite phase
obtained in these samples is rich in Ni, Mo, and Ti, as shown
in the EDS maps. Figure 12(a) shows that for aging tempera-
tures ranging from 460 to 490 °C, the highest and lowest
Int J Adv Manuf Technol (2021) 115:3999–4020
hardness values were obtained at 480 °C for 8 h. The highest
hardness value of 56.42 ± 1.12 HRC corresponds to sample D,
fabricated with an energy density of 36.90 J/mm2, and the
lowest hardness value of 53.87 ± 1.26 HRC corresponded to
sample B, fabricated with an energy density of 55.94 J/mm2.
On the other hand, the aging heat treatment of 530 °C for 1 h
evidenced the lowest hardness value of 52.28 ± 0.89 HRC,
corresponding to sample C, fabricated with an energy density
of 36.90 J/mm2. The hardness decrease obeys to the fact that
above 500 °C, the formation of austenite by diffusion and the
amount of austenite formed during aging are totally or partial-
ly retained at room temperature, depending on the chemical
composition; e.g., if the Ni content is high, the austenite is
more stable.
To explain the phenomenon of austenite observed in as-
built condition samples, the authors propose the graphic
sketch showed in Figs. 17 and 18. Therefore, the phenomenon
can be discussed as follows.
Assuming that (i) the deposit thickness change Δx is the
same for both deposition conditions (with rotation and without
rotation, ΔxNR ≈ ΔxR) for each energy density and (ii) the
outer and inner surfaces of the deposits (see Fig. 17) achieve
a homogenous temperature along the whole surface (T2 and
Int J Adv Manuf Technol (2021) 115:3999–4020 4013

60 32
55.94 J/mm2
(Non-rotated)
HARDNESS
SAMPLE A b)
SAMPLE B 28
55 SAMPLE C
SAMPLE D
55.94 J/mm2
(Rotated) 24
Hard ne ss (HRC)

50

Austenite (%)
20
2
36.90 J/mm
(Non-rotated)
45 16

c)
36.90 J/mm2
(Rotated) 12
40

8
AUSTENITE
35 SAMPLE A
SAMPLE B 4

a) SAMPLE C
SAMPLE D
30 0
AS-BUILT 460/8 480/6 480/8 490/4 530/1

Heat treatments (°C/h)

Fig. 12 a) Hardness and austenite phase fraction of 18Ni300 MS fabricated by LC as a function of different heat treatment conditions, b) building pattern
between layers without rotation, and c) building pattern between layers rotating 90°

T1, respectively). These conditions would guarantee that a region below the curve) which acts as thermal treatment de-
unidirectional heat flux takes place during deposition accord- creases with time as is sketched in Fig. 17. Moreover, it is
ing to: expected that the amount of heat accumulated during the de-
  position time would be directly proportional to the reversed
ΔT J
q” ¼ k ð7Þ austenitic phase content in the final deposit. Therefore, an
Δx m2 s increasing austenitic content is related to a larger heat accu-
mulation, i.e., a larger area below the curve (see Fig. 17).
where k is the thermal conductivity (J/s K−1 m−1), q” is the
Based on Fig. 17, the aforementioned mechanisms and
heat flux (J/m2 s−1), ΔT is the temperature change (K), and Δx
assumptions, the differences in the austenite phase content
is the deposit thickness change (m).
estimated by the Rietveld analysis, can be rationalized as fol-
According to Gedda et al. [50], power lost by convection
lows by the graphical sketch of Fig. 18.
occurs between the interaction of the molten pool and the
Figure 18a represents the deposition time (tD) for each lay-
shielding gas, and power lost by convection represents 0.1%
er. It is observed that for samples with rotation, the deposition
of the output power of the laser, which is considered negligi-
time for the even layers (tD2, tD4, and tD6) is greater than the
ble and it can be ignored as well as power losses due to radi-
time for the odd layers (tD1, tD3, and tD5), thus increasing the
ation and power absorbed by powder particles that do not
total deposition time in the rotated samples due to the increase
enter the molten pool [50]. From the above, we consider that
in the idle laser time for the even layers (deposition parallel to
the shielding gas does not affect the heat transfer during the
the width of the fabricated sample). In other words, the rotated
process and can be ignored for the heat transfer analysis of Eq.
samples have a greater heat dissipation time, which can result
7.
in a lower temperature at the substrate/deposit interface (T1) as
During the deposition, the number of layers increases, and
is represented in Fig. 18a. As a consequence, a smaller ΔT
consequently, the total Δxn is greater; in contrast, the ΔT
would be expected for the rotated samples. Another aspect
becomes smaller with the heat accumulation into the deposited
that contributes to heat dissipation is the thermal conductivity
system (substrate+deposited layer) and, therefore, the total
(K), which for 18Ni-300 MS has been reported to increase
heat received in the deposited system by unit area (the dashed
linearly with temperature in the range from 20 to 1300 °C
4014 Int J Adv Manuf Technol (2021) 115:3999–4020

Fig. 13 (a) XRD patterns of samples A–D in as-built condition, (b) intensities in the peak γ (111) of the austenite in as-built condition, (c) XRD patterns
of samples A–D with an aging treatment at 480 °C during 6 h, and (d) intensities in the peak γ (111) of the austenite in aging condition

[51]. It is expected that the thermal conductivity behaves sim- On the other hand, the experimental evidence showed that
ilarly to that described by the drawing in Fig. 18c for both non-rotated samples have a higher amount of the austenite
printing strategies. Therefore, a higher thermal conductivity phase (Fig. 12(a)), independent of the density energy
values for the non-rotated samples can be expected. employed during fabrication, resulting in an overaging caused

Fig. 14 a Optical microscope image of sample A in as-built condition, b–d SEM images of sample A in as-built condition, e optical microscope image of
sample D in as-built condition, f–h SEM images of sample D in as-built condition
Int J Adv Manuf Technol (2021) 115:3999–4020
Fig. 15 a SEM images and EDS
mapping of sample A in as-built
condition and b SEM images and
EDS mapping of sample D in as-
built condition
by the intrinsic heat treatment received during the deposition
of layers. These experimental results suggest that the amount
of heat per unit area received during the deposition time (i.e.,
area under the curve) by the non-rotated samples should be
greater than that received by the rotated samples, q"NR55.94 >
q"R55.94 > q"NR36.90 > q"R36.90, as sketched in Fig. 18d. This
analysis also suggests that ΔT has a greater significance than
the thermal conductivity within our experimental window.
Since samples fabricated with an energy density of 36.90
J/mm2 can be expected to have smaller areas than those with
55.94 J/mm2, these should also present a lower degree of
4015
overaging and, therefore, a lower amount of the austenite
phase. Moreover, the deposition times were shorter in the
samples of low energy density, and the idle laser times were
longer, as shown in Fig. 18d and Table 4, comparing each
deposition conditions. This observation is in agreement with
Costa et al. [52] who showed that a lower percentage of the
austenite phase is obtained when a long idle time occurs be-
tween deposited layers (Δt ≥ 10 s) due to the temperature of
each layer of material decreases below Ms before a new layer
is deposited, allowing austenite to transform to martensite.
Also, Costa et al. [53] demonstrated that for short idle times,
4016
Fig. 16 a SEM images and EDS
mapping of sample A aged at 480
°C during 6 h and b SEM images
and EDS mapping of sample A
aged at 530 °C during 1 h
the martensitic transformation only occurs after completion of
the part, when it cools to room temperature.
Lower contents of austenite phase in as-built conditions of
18Ni-300 MS have been reported by LPBF processes. Casati
et al. [14] reported 11.38%, Jägle et al. [18] reported 8.5%,
Kempen et al. [9] reported 5.8%, Suryawanshi et al. [7] re-
ported 10%, and Tan et al. [10] reported 10.3%. Cooling rates
during the LPBF processes are relatively high (~108 °C/s).
Therefore, the microstructure in the process consists mainly
of martensite, with a small austenite content. Conversely, LC
has slower cooling rates (~104 °C/s), and because of the larger
heat input on the melt and the accumulated heat between
Int J Adv Manuf Technol (2021) 115:3999–4020
layers, it can be assumed that the tracks remain close or even
surpass the initial transformation temperature to austenitic
phase As, 650 °C [8], 666 °C [13], and 600 °C [49].
Moreover, regarding the Ni content of 18Ni-300 MS, the aus-
tenite becomes stable at room temperature, being this the lead-
ing cause of high austenitic content in the as-built condition
samples.
Moreover, mechanical and metallurgical properties that
characterize the maraging steel are achieved after aging heat
treatments. These promote the formation of Ni3(Mo, Ti) and
Fe2Mo precipitates, which are diffusely distributed within the
grain and in the lath martensite grain boundaries [48]. In Fig.
Int J Adv Manuf Technol (2021) 115:3999–4020 4017

Fig. 17 Representative diagram

of heat accumulation during
layer-by-layer deposition

Fig. 18 a Deposition time per

layer, b heat dissipation of rotated
and non-rotated samples, c ther-
mal conductivity as function of
temperature, d amount of heat re-
ceived per unit area during the
deposition time, and e austenite
phase as function of heat
accumulation
4018
12(a), the highest content of austenite phase is obtained after
the aging heat treatment at 530 °C for 1 h, in comparison with
Casati et al. [14] in which the maximum value was obtained at
540 °C for 8 h. Additionally, Banerjee [35] mentioned that
aging for a prolonged period of time at a temperature higher
than 550 °C may lead to formation of high alloy austenite; Zhu
et al. [49] mentioned that aging between 500 °C and the As
temperature produces austenite precipitation by a diffusion
controlled action due to an overaging. Above ~ 500 °C, the
austenite phase formation is diffusion-controlled. During ag-
ing, the temperature must be kept below 500 °C to avoid the
reverse reaction and austenite formation. On the other hand, in
the aging heat treatments carried out below 500 °C, the highest
content of austenite obtained was 5.33 wt%, which is slightly
lower than reported by LPBF processes; Casati et al. [14]
reported 15.55% with optimal aged heat treatment, Jägle
et al. [18] reported 16.5%, Kempen et al. [9] obtained 9.4%,
Suryawanshi et al. [7] reported 15%, and Tan et al. [10] ob-
tained 11%.
Overall, the contour and overlaid plots provide a useful
analysis of the influence of the parameters and process opti-
mization on improving the deposited geometry of the MS
track for 2D and 3D LC applications, which can range from
applications of structural component for LC manufacturing to
the repair of high-value tooling for MRO and heavy indus-
tries. The processing map is a reliable reference value for a
constant powder feed rate of 14 g/min, and further research is
needed to evaluate the robustness of them at different powder
feed rates. Likewise, depending on the application, selecting
suitable heat treatment plays a significant role since high
levels of hardness with good ductility can be achieved by
controlling the austenite content, leading to an increase in
the use of 18Ni-300 MS instead of carbon hardened steels.
Future works will analyze mechanical and tribological prop-
erties produced with optimized parameters.
4 Conclusions
This section summarizes the main accomplishments
concerning the influence of the process parameters on the
geometry control of the 18Ni-300 MS tracks deposited by
LC technology as well as on microstructure, under different
heat treatments:
& Although the three studied key process parameters have
an influence on track geometry, laser power has the most
statistically significant effect on dilution, whereas velocity
is the most statistically significant parameter influencing
height, width, depth, and porosity.
& For high laser power settings, decreasing spot size pro-
duces a significant increase in dilution, despite the in-
crease in energy density being relatively small, which
Int J Adv Manuf Technol (2021) 115:3999–4020
might have occurred due to a combined effect of higher
power density with a higher peak value on the crest of the
energy distribution of the Gaussian-like beam.
& Processing maps to optimize the geometrical characteris-
tics and dilution of the tracks were successfully developed
and experimentally validated: (i) the higher tracks with
low dilution corresponded to a laser power of 800 W, a
velocity of 5 mm/s, and a laser spot size of 2.86 mm and
(ii) wider tracks with low dilution corresponded to a laser
power of 950 W, a velocity of 8.8 mm/s, and a laser spot
size of 2.86 mm.
& At the optimal processing regions for manufacturing and
repair (see Figs. 11 and 12), no significant effect was ob-
served on the hardness behavior independently of the ag-
ing treatment used.
& An increase in the austenite content was observed at tem-
peratures above or equal to 480 °C with the aging time.
This result may favor the ductility of the manufactured and
repaired parts of 18Ni300 maraging steel.
& The observed differences in the austenitic content among
rotated and non-rotated as-built samples look to be direct-
ly related to available time to dissipate the accumulated
heat after each layer deposition. Rotated samples had
higher idle times for the even layers, allowing the samples
to retain more of the martensite formed during layers
solidification.
Authors’ contribution Not applicable
Funding We are grateful to CENAPROT, CONACyT (Consejo
Nacional de Ciencia y Tecnología) and the Agencia Espacial Mexicana
for financing this study through project num. 275781. Thanks are also due
to the Conacyt Consortium in Additive Manufacturing (CONMAD) for
the use of its experimental facilities for this research, and to CONACyT
for its financing through the programs FORDECYT (projects 297265 and
296384). Author Juansethi Ibarra-Medina acknowledges the support of
CONACYT through Fellowship at the Center for Engineering and
Industrial Development (CIDESI) (Project: Catedras 2017—num. 57).
Availability of data and material Not applicable
Code availability Not applicable
Declarations
Conflict of interest The authors declare no competing interests.
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