j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 1 : 3 7 3 e3 8 7

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Original Article

Effect of atmospheric-controlled induction-heating

fine particle peening on wear resistance and
fatigue properties of maraging steel fabricated by
laser powder-bed fusion

Shogo Takesue a,*, Atsushi Ezura b, Yusuke Maki c, Motoaki Hayama c,

Yoshitaka Misaka d, Jun Komotori e
a
Department of Mechanical Engineering, Kyoto Institute of Technology, Matsugasakigoshokaidocho, Sakyo-ku,
Kyoto-shi, Kyoto, 606-8585, Japan
b
Faculty of Engineering, Sanjo City University, 1341 Kamisugoro, Sanjo-shi, Niigata, 955-0091, Japan
c
Graduate School of Science and Technology, Keio University, 3-14-1 Hiyoshi, Kohoku-ku, Yokohama-shi,
Kanagawa, 223-8522, Japan
d
Neturen Co., Ltd., 7-4-10 Tamura, Hiratsuka-shi, Kanagawa, 245-0013, Japan
e
Department of Mechanical Engineering, Keio University, 3-14-1 Hiyoshi, Kohoku-ku, Yokohama-shi, Kanagawa,
223-8522, Japan

article info abstract

Article history: Maraging steel components fabricated by laser powder-bed fusion, which is a technique of
Received 18 August 2022 additive manufacturing, are expected to be used widely because of their high strength,
Accepted 10 September 2022 hardness and toughness. To apply maraging steel manufactured by laser powder-bed
Available online 15 September 2022 fusion in wider industrial fields and prevent the components from fracture, a study was
conducted to improve the wear resistance and fatigue properties of the steel by an
Keywords: atmospheric-controlled induction-heating fine particle peening surface modification
Surface modification technique. The technique developed can create hard intermetallic compound layers and
Maraging steel introduce peening effects, which are expected to improve the wear resistance and fatigue
Laser powder-bed fusion properties of maraging steel fabricated by laser powder-bed fusion. The prepared speci-
Wear resistance mens were examined using optical microscopy, scanning electron microscopy, energy
Fatigue property dispersive X-ray spectroscopy, laser microscopy, X-ray diffraction, micro-Vickers hardness
testing, nano-indentation testing, reciprocating ball-on-disk wear tests and axial fatigue
tests. It was revealed that atmospheric-controlled induction-heating fine particle peening
using mechanically milled particles formed FeeAl intermetallic compound layers with
high hardness, introduced compressive residual stresses and increased the hardness of the
maraging steel substrate owing to age hardening. In conclusion, atmospheric-controlled
induction-heating fine particle peening can simultaneously improve the wear resistance
and fatigue properties of maraging steel fabricated by laser powder-bed fusion within a few
minutes. These achievements can expand applications of maraging steel fabricated by
laser powder-bed fusion.

* Corresponding author.
E-mail address: stakesue@kit.ac.jp (S. Takesue).
https://doi.org/10.1016/j.jmrt.2022.09.046
2238-7854/© 2022 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).
374 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 1 : 3 7 3 e3 8 7

© 2022 The Author(s). Published by Elsevier B.V. This is an open access article under the CC
BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

maraging steel components fabricated by LPBF have been

1. Introduction assessed. Yin et al. [10] reported that the wear resistance of
such items could be improved by aging under optimal condi-
Maraging steel is a precipitation-strengthened alloy possess- tions, as a consequence of increased hardness. Podgornik
ing high strength, hardness and toughness. It is widely used in et al. [11] studied the dependence of the wear resistance of the
the aircraft, aerospace and tooling industries. Recently, laser steel on the building direction and heat treatment. Bae et al.
powder-bed fusion (LPBF) has received significant attention as [12] examined that the effect of solution treatment, counter-
a means of fabricating various components from this mate- part material and wear loads on wear behavior. In contrast,
rial. In LPBF, a laser beam is used to melt a powder feedstock Croccolo et al. [13,14] investigated the effects of building di-
selectively on a substrate based on a sliced three-dimensional rection and machining on the fatigue properties of maraging
model generated using computer-aided design. Thin layers of steel fabricated by LPBF. Meneghetti et al. [15] demonstrated
powder are repeatedly deposited using this technique, and that the fatigue strength of maraging steel components pro-
items with complex and near-net shapes, which are difficult duced using LPBF was lower than that of vacuum-melted
to fabricate using conventional manufacturing methods, can maraging steel because of the fatigue crack initiation that
be produced. As an example, LPBF can be used to fabricate resulted from a lack of fusion defects. Uematsu et al. [16]
complex molds made of maraging steel that contain highly
efficient internal cooling channels. The LPBF process has been
investigated in several studies using maraging steel, such as
optimization of the processing parameters based on a statis-
tical approach [1] and the construction of a process map [2].
The effects of these parameters on the microstructure and
mechanical properties were also investigated, and it was
found that low and high laser power, scanning speed and
scanning space all reduced the relative density [3], and the
porosity in parts had the greatest effect on the mechanical
properties [4]. The aging of maraging steel fabricated by LPBF
promoted an increase in strength but a decrease in ductility
[5], and the aging parameter could be tailored to adjust
strength, ductility and anisotropy [6]. Detailed microstructure
observation revealed that an LPBF-fabricated sample exhibi-
ted the characteristic melt pools which were mainly consisted
of a lath martensite structure with a high density of disloca-
tions [7], and the as-built maraging steel had a well-made
cellular structure [8]. Moreover, a novel maraging steel
Fig. 1 e SEM image of raw maraging steel powder.
developed for the LPBF process was also developed and
characterized [9].
For components made of maraging steel fabricated by LPBF
to be used widely, such properties as wear and fatigue must be
clarified and improved to prevent damage and fracture. In
several studies, the wear resistance and fatigue properties of

Table 1 e Previous studies about maraging steel

fabricated by LPBF.
Optimization of the processing parameters [1,2]
Investigation of microstructure and mechanical properties [3,4]
Aging behavior [5,6]
Detailed observation of microstructure [7,8]
Development and characterization of a novel maraging [9]
steel
Investigation of the wear behavior [10e12]
Investigation of the fatigue properties [13e16]
Surface modification of maraging steel [17e20]

Fig. 2 e Specimen configuration for fatigue tests.

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Fig. 3 e AIH-FPP systems used to process (a) disk-shaped and (b) fatigue specimens.
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FPP can simultaneously and rapidly improve the wear resis-

Table 2 e Conditions applied during the AIH-FPP
tance and fatigue properties of maraging steel items produced
processing of disk-shaped specimens.
by LPBF.
Atmosphere Nitrogen (Purity of 99.99%)
Based on this background, the research target of this study
Particle supply rate 1 g /s was the rapid improvement of the wear resistance and fatigue
Peening time 120 s properties of maraging steel fabricated by LPBF to prevent
Temperature T 673, 723, 773, 873, 1073 K
fractures of components made of the steel in service because
Heating time after FPP t 0, 120, 240 s
Gas flow rate 130 L/min
previous studies about surface modification of metals fabri-
Nozzle distance 100 mm cated by LPBF addressed either wear or fatigue. To achieve the
Internal diameter of nozzle 6 mm objective, the developed AIH-FPP was applied because the
surface modification technique can create hard intermetallic
revealed that specimens with a hybrid structure, which con- compound layers and provide peening effects. The effects of
sisted of LPBF parts on a conventionally manufactured base temperature and heating time after FPP on the surface char-
plate, had lower fatigue strength than conventionally manu- acteristics of the steel were investigated. The wear resistance
factured maraging steel. and fatigue properties of the AIH-FPP-treated specimens were
Surface modifications can be used to improve the wear also evaluated and are discussed herein.
resistance and fatigue strength of metallic materials.
Increasing the surface hardness of metals by forming hard-
ened layers is known to improve wear resistance. Godec et al. 2. Experimental procedures
[17] revealed that the wear resistance of maraging steel
fabricated by LPBF increased with higher nitriding tempera- AIH-FPP is expected to improve the wear resistance and fa-
ture where thicker compound layer formed. In addition, the tigue properties of maraging steel fabricated via LPBF by
fatigue properties of metals can be enhanced by applying creating a hard intermetallic compound layer and introducing
various peening techniques owing to work hardening and the a peening effect. To examine the effect of AIH-FPP, the ex-
introduction of compressive residual stress. The fatigue periments explained in this section were performed.
properties of maraging steel items fabricated by LPBF have
also been improved using shot peening [18], vibratory finish- 2.1. Material and specimens
ing [19] and laser peening [20]. Table 1 summarizes the pre-
vious studies about maraging steel fabricated by LPBF. Specimens made of maraging steel manufactured by LPBF
Although the effects of surface modification on the properties were prepared so that AIH-FPP, surface characterizations,
of other metallic materials fabricated by LPBF, such as wear tests and fatigue tests could be performed. Maraging
aluminum alloy [21], titanium alloy [22] and stainless steel steel powders with a diameter of 10e50 mm and an average
[23], have been investigated previously, simultaneous im- diameter of 30 mm were supplied by Sodick Co., Ltd., Japan, for
provements of the wear resistance and fatigue properties of use as the raw material (ULTRA 21). Fig. 1 presents a scanning
LPBF-fabricated metals were not achieved. In addition, con- electron microscopy (SEM) image of the raw powder. Bars,
ventional heat treatments generally take a long time to each having a diameter of 20 mm and a length of 150 mm,
complete. were fabricated from this powder using an LPBF apparatus
Atmospheric-controlled induction-heating fine particle (OPM-250L, Sodick Co., Ltd., Japan). These bars were formed in
peening (AIH-FPP) is a surface modification technique previ- the vertical direction relative to the orientation of the base-
ously developed by the authors. This process is capable of plate under a nitrogen atmosphere. Fabrication was done with
simultaneously improving the wear resistance and fatigue a laser power of 420 W, laser wavelength of 1064 nm, spot
properties of maraging steel items produced by LPBF and so diameter of 0.2 mm, scanning speed of 1000 mm/s, hatching
could be applied for this purpose. In the AIH-FPP technique, pitch of 0.15 mm, layer thickness of 50 mm and rotation angle
fine particle peening (FPP) involving collisions with high- between layers of 1.57 rad (90
). Relative density measure-
velocity fine particles (<200 mm in diameter) is applied to an ments using the Archimedes method showed that the relative
induction-heated metal specimen under a controlled atmo- density of the fabricated samples was 99.7%, indicating that
sphere [24,25]. During this process, elements contained in the dense specimens could be manufactured by LPBF under the
shot particles are transferred to the surfaces of the treated conditions applied.
material, where they subsequently react with other elements Some of the manufactured bars were machined into disk-
in both the shot particles and the substrate to form a hard shaped specimens, each having a diameter of 15 mm and a
layer of intermetallic compounds on the treated surfaces thickness of 4 mm, for surface characterization and wear tests.
within several minutes, such as a TieAl layer on carbon steel One end surface of each specimen was polished using emery
[26], a TieAl layer on titanium alloy [27] and an FeeAl layer on paper (#240-#1200). The remaining bars were machined into
stainless steel [28]. The rapid generation of these intermetallic the configuration shown in Fig. 2 for fatigue tests. The surfaces
compounds is attributed to combustion synthesis reactions of these specimens were polished using emery paper (#100-
on the treated surfaces [27]. Moreover, AIH-FPP can have #2000) and an alumina suspension with a particle diameter of
various peening effects, such as increasing the surface hard- 3 mm to obtain a mirror finish. Some of the disk-shaped speci-
ness, generation of compressive residual stress and grain mens and fatigue specimens were heated at 753 K for 10.8 ks to
refinement, all of which may enhance the fatigue properties of simulate aging, using an electric furnace. After heating, the
low-alloy steel [29]. These previous studies suggest that AIH- specimens were air-cooled to room temperature.
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For comparison purposes during the fatigue testing trials, heating time was increased from 10 to 20 s, while the peening
maraging steel samples were also fabricated by rolling, and time was increased from 120 to 240 s. Based on the analysis of
machined into the same configuration shown in Fig. 2, after results for the disk-shaped specimens (see Sections 3.1 and
which each specimen was polished to a mirror finish. Some of 3.2), the temperature and heating time after FPP for these
these rolled specimens were aged using the same procedure samples were determined to be 723 K and 0 s, respectively.
as applied to the specimens fabricated by LPBF. The temperature of each specimen surface during AIH-FPP
was measured using K-type thermocouples and controlled
2.2. AIH-FPP by adjusting the power applied to the inverter.
To create hard FeeAl intermetallic compound layers,
To achieve surface modification of the maraging steel fabri- which improved the wear resistance of stainless steel in a
cated by LPBF, AIH-FPP was applied to one surface of each previous study [28], on maraging steel fabricated by LPBF, the
disk-shaped specimen and to the round areas of the fatigue shot particles in these trials were prepared by mechanically
specimens. Fig. 3(a) and (b) are diagrams of the AIH-FPP sys- milling a mixture of high-speed tool steel particles and pure
tems used to process the disk-shaped and fatigue specimens, aluminum particles. A 100 g quantity of steel particles with
respectively. Both systems included a nozzle and an diameters of 75e125 mm and 10 g of pure aluminum particles
induction-heating coil in a chamber, the internal atmosphere with an average diameter of 30 mm were transferred into a
of which could be replaced by supplying gas through a nozzle. zirconia pot along with 1 mL of isopropanol (purity of 99.5%,
The AIH-FPP system for disk-shaped specimens also included SigmaeAldrich Co. LLC, USA) to prevent coarsening of the
a vacuum pump, and the chamber was evacuated to approx- particles [31]. The pot was inserted into a container made of
imately 0.05 MPa before the gas was introduced. The system stainless steel, and the atmosphere inside the container was
for the fatigue specimens included a lathe to rotate the sam- replaced with argon. Mechanical milling was subsequently
ples so that the entire surface of the round area was treated. performed at a rotation rate of 6.7/s (400 rpm). A total of 72
Table 2 summarizes the AIH-FPP conditions, while Fig. 4(a) milling cycles were performed, with one cycle consisting of
presents the thermal history associated with the AIH-FPP milling for 300 s followed by a 900 s pause. Following this
treatment of the disk-shaped specimens. The temperature, T process, the product was sieved, and particles with diameters
in Fig. 4(a), and heating time following FPP, t in Fig. 4(a), were of 75e150 mm were captured for use as AIH-FPP shot particles.
varied, and both affected the formation of the surface- When hard particles are mechanically milled with soft
modified layer during AIH-FPP [30]. The thermal history of particles, thin layers of the soft material form on the surface of
the fatigue specimens is shown in Fig. 4(b). Because of the the hard particles [32e34]. Fig. 5 shows an SEM image and
larger volume and surface area of the latter specimens, the elemental maps acquired by energy dispersive X-ray spec-
troscopy (EDX) of a particle generated by this procedure.

2.3. Characterization of specimens

Various microstructural characterizations of the prepared

specimens were performed to investigate the effect of AIH-FPP
on the surface properties of maraging steel fabricated by LPBF.
Cross-sections of the steel specimens were analyzed using
optical microscopy, SEM and EDX. Prior to these observations,
the specimens were cut, covered with a phenolic resin and
polished to a mirror finish using emery paper and an alumina
suspension. Etching using nital (a mixture of 5 mL of nitric
acid (purity of 60.0%e61.0%, Kanto Chemical Co., Inc., Japan)
and 95 mL of ethanol (purity of 99.5%, SigmaeAldrich Co.
LLC, USA)) was also performed prior to observations using
optical microscopy. The compounds formed on the specimens
were identified using X-ray diffraction (XRD) with Cr Ka radi-
ation (wavelength of 0.154 nm), at a current of 40 mA and a
voltage of 40 kV. The roughness values for the fatigue speci-
mens were determined using laser microscopy. The average
surface roughness, Ra, was obtained based on the assessment
of a length of 1000 mm. Vickers hardness values were
measured using a micro-Vickers hardness tester at a force of
0.98 N with a hold time of 15 s. Cross-sectional distributions of
hardness and Young's modulus were ascertained by nano-
indentation at a force of 0.1 mN. The residual stresses gener-
ated in the longitudinal direction of the fatigue specimens
Fig. 4 e Thermal histories during AIH-FPP processing of (a) were calculated based on XRD data and the cosa method for a-
disk-shaped and (b) fatigue specimens. Fe (211) planes, 2q ¼ 2.73 rad (156.4
), with Cr Ka radiation at
30 kV and 1.5 mA. The incident X-ray angle was 0.61 rad (35
).
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Fig. 5 e (a) SEM micrograph and (b) Fe and (c) Al maps of steel/aluminum particle obtained by mechanical milling.

2.4. Wear and fatigue testing effect, which improve the wear resistance and fatigue prop-
erties of maraging steel fabricated by LPBF. To determine the
Wear and fatigue tests were performed to examine the effect influence of AIH-FPP using mechanically milled particles on
of AIH-FPP on the wear and fatigue properties of maraging the surface, wear and fatigue properties, in this section, the
steel fabricated by LPBF. Reciprocating ball-on-disk wear tests obtained results are presented and discussed.
were performed using disk-shaped specimens at room tem-
perature in air. These tests were conducted using an alumina 3.1. Effect of temperature and heating time after FPP on
ball with a diameter of 3 mm as the opposing material, a force formation of surface-modified layer
of 1 N, a sliding stroke of 8 mm, a sliding speed of 10 mm/s
and a sliding distance of 224 m. The mass of each specimen To assess the effect of the AIH-FPP temperature on the surface
was measured before and after the trial using an electric characteristics of maraging steel items fabricated by LPBF, the
balance to make it possible to determine the wear loss during disk-shaped specimens were treated with AIH-FPP at several
each test. The crossesectional profiles of the wear tracks temperatures with a post-FPP heating time of 120 s, and the
formed on the specimens were assessed using laser micro- resulting surfaces were analyzed. Fig. 6 shows SEM micro-
scopy. Axial fatigue tests were conducted with a hydraulic graphs and EDX maps of the longitudinal cross-sections of
servo fatigue testing machine at room temperature under these samples. The analyses found Al on the surfaces of all
atmospheric conditions. The tests were performed at a fre- specimens, and the thickness of this Al layer increased with
quency of 10 Hz and a stress ratio of 1. After each trial, the increasing temperature during AIH-FPP. When FPP is per-
fracture surfaces of the failed specimen were analyzed using formed using mechanically milled particles, the elements on
SEM and EDX. the particle surfaces are transferred to the substrate being
treated [35]. Moreover, the amount of transferred material
increases with increasing processing temperature [25].
3. Results and discussion Therefore, employing shot particles coated with a thin Al layer
provides an Al coating to the steel, and the thickness of this
AIH-FPP is expected to create a surface modified layer con- layer increases with increasing AIH-FPP temperature. In
sisting of intermetallic compounds and introduce peening addition, Fe was detected in the same regions in which Al was

Fig. 6 e SEM micrographs and EDX maps of longitudinal cross-sections of disk-shaped specimens subjected to AIH-FPP at
various temperatures.
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Fig. 8 e Vickers hardness measured in substrate regions of

disk-shaped specimens before and after processing with
AIH-FPP at various temperatures (n ¼ 20, mean ± SD).

thickness of approximately 10e20 mm were created, and

Fe2Al5 formed on the treated surfaces [28]. This indicates that
AIH-FPP using mechanically milled particles can create an
intermetallic compound layer regardless of the steel type. In
addition, the specimens processed with AIH-FPP at tempera-
tures of 673e773 K produced g-Fe (austenite) as well as a-Fe
peaks. Casati et al. [5] demonstrated that martensite in mar-
aging steel items fabricated by LPBF can revert to austenite
upon heating at 733e873 K. Although the temperatures in this
study were somewhat lower than those assessed by Casati
et al., the transition of martensite to austenite in maraging
steel would be expected to occur during the heating process
associated with AIH-FPP. This indicates that AIH-FPP should
modify both the surface and substrate characteristics of
maraging steel.
To investigate the effect of AIH-FPP on the hardness of
treated maraging steel substrates, the Vickers hardness for
original maraging steel and the various treated specimens
was measured. Fig. 8 provides the results of these evalua-
Fig. 7 e XRD patterns obtained from disk-shaped
tions, which indicate that materials processed using AIH-FPP
specimens as-built and subjected to AIH-FPP at various
at 673, 723 and 773 K exhibited a higher hardness than the
temperatures.
as-built material, whereas the specimens treated at 873 and
1073 K were found to have a lower hardness than the as-
built material. Each of the specimens processed with AIH-
observed. These results imply that Al from the shot particles FPP at 673, 723 and 773 K formed an austenite phase (as
reacted with Fe in the steel substrate. shown in Fig. 7) that would be expected to reduce the
The compounds formed on the specimen surfaces were hardness of the material. However, the measured hardness
analyzed using XRD. Fig. 7 provides the resulting diffraction values of these materials were higher than that of the as-
patterns. The as-built specimen only generated a-Fe peaks built specimen. Yin et al. [10] reported that the aging
(attributed to martensite), whereas all the AIH-FPP-treated behavior of maraging steel depends on the heating temper-
specimens provided peaks resulting from FeeAl interme- ature and that the highest hardness and ultimate tensile
tallic compounds, such as Fe2Al5. These results demonstrate strength could be obtained at 763 K. The hardness values for
that layers of FeeAl intermetallic compounds were formed on the specimens treated with AIH-FPP at 673, 723 and 773 K
the steel surfaces by AIH-FPP using mechanically milled par- increased because of age hardening and the precipitation of
ticles, indicating that the transferred Al reacts with Fe con- intermetallic compounds, such as Ni3Ti, Ni3Mo and Fe2Mo
tained in the substrate, even though the heating time was [3]. The Vickers hardness of maraging steel fabricated by
short. The formation of this compound layer within a span of LPBF and aged under the optimal condition was more than
time of only several minutes is ascribed to the occurrence of a 600 HV; therefore, the AIH-FPP-treated specimens did not
combustion synthesis reaction between Fe and Al [36] and to exhibit the maximum hardness of aged maraging steel
local increases in temperature at the treated surface. When owing to the short heating time. The hardness values of the
AIH-FPP using the same mechanically milled particles was specimens treated with AIH-FPP at 873 and 1073 K were
performed for stainless steel, Al transferred layers with a lower than that of the as-built specimen. Yin et al. [10]
380 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 1 : 3 7 3 e3 8 7

Fig. 9 e SEM micrographs and EDX maps of longitudinal cross-sections of disk-shaped specimens processed with AIH-FPP
when various heating times were applied after FPP.

determined that heating at higher temperatures, such as the lowest hardness and Young's modulus, while the highest
863 K, caused over-aging and reduced the hardness of values are found in the inner region (layer B). Both the hard-
maraging steel because of the decomposition of intermetallic ness and Young's modulus gradually decrease with a further
compounds. Therefore, the specimens treated using AIH-FPP increase in the distance from the surface (layers C and D), and
at 873 and 1073 K in the present work probably underwent both values eventually return to those for the steel substrate.
over-aging and thus had reduced hardness. These results indicate that the chemical composition and
The effect of heating time after FPP on the characteristics mechanical properties inside the surface-modified layer vary
of the surface-modified layers was assessed by performing with depth.
AIH-FPP at 1023 K with heating times of 0, 120 and 240 s. Here, Varying the heating time was found to change the thick-
a heating time of 0 s indicates that the specimen was imme- nesses of layers B, C and D, all of which contained transferred
diately cooled after being subjected to FPP at 1023 K for 120 s. Al, as shown in Fig. 9. The mechanical properties determined
Fig. 9 presents SEM micrographs and EDX maps of longitudi- by the nano-indentation tests (Fig. 10) demonstrated that the
nal cross-sections of disk-shaped specimens treated with outermost layer (layer A) had the lowest hardness and Young's
AIH-FPP while different heating times were applied after FPP. modulus and was clearly made of unreacted Al. The layer B,
It is evident that the thickness of the layer containing Al is which exhibited the highest hardness and Young's modulus,
almost independent of the heating time. However, the SEM probably consisted of Fe2Al5. This is one of the hardest FeeAl
micrographs indicate four distinct layers (referred to herein as intermetallic compounds [37]. This hypothesis was confirmed
layers A, B, C, and D) and show that the thickness of layers C by the XRD pattern presented in Fig. 7. Layer B also exhibited
and D increases with increasing heating time. Moreover, in an increasing number of voids as the heating time after FPP
the case of layer B, voids are formed with increasing heating was prolonged. These are believed to have been Kirkendall
time. voids that formed as a result of the different diffusion rates of
The layers formed on these metal samples were also Fe and Al atoms in the metal and the resulting accumulation
characterized by measuring the hardness and Young's of atomic vacancies. Layers C and D, in which both the hard-
modulus using nano-indentation. Fig. 10 shows the cross- ness and Young's modulus gradually decreased, are thought
sectional distributions of these data for a disk-shaped spec- to comprise Fe-rich FeeAl intermetallic compounds, such as
imen treated with AIH-FPP with a heating time after FPP of FeAl and Fe3Al, which are known to be less hard than Al-rich
120 s. The outermost surface of the specimen (layer A) exhibits FeeAl intermetallic compounds [37].
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 1 : 3 7 3 e3 8 7 381

Fig. 11 e Wear losses for as-built specimen, LPBF þ aged

specimen, and specimens subjected to AIH-FPP at different
temperatures (n ¼ 3, mean ± SD).

formation of a layer of FeeAl intermetallic compounds

improved the wear resistance of maraging steel items fabri-
cated by LPBF.
As indicated in Figs. 11 and 12, the LPBF þ aged specimen
exhibited higher wear resistance than the as-built specimen
as a consequence of the age hardening of the former. Both
specimens subjected to AIH-FPP (at 723 or 1073 K) showed
higher wear resistance than the LPBF þ aged sample. This
finding indicates that the formation of a layer of FeeAl inter-
metallic compound improved the wear resistance of samples
fabricated by LPBF to a greater extent than aging. This enables
Fig. 10 e Cross-sectional distributions of (a) hardness and the hardness to be increased by AIH-FPP in conjunction with a
(b) Young's modulus for disk-shaped specimens processed shorter processing time of several minutes compared with
with AIH-FPP using a heating time of 120 s (n ¼ 20, several hours of aging. The specimen processed by AIH-FPP at
mean ± SD). 723 K also showed higher wear resistance than that treated at
1073 K. According to the nano-indentation data shown in
Fig. 10, the surface of the latter metal had a low hardness layer
3.2. Effect of AIH-FPP on wear resistance of maraging of unreacted aluminum. Wear of the AIH-FPP-treated speci-
steel specimens fabricated by LPBF mens occurred at surface asperities that were locally worn as
a result of contact with the counter material [38]. It is apparent
The effect of AIH-FPP on the wear resistance of the steel that the unreacted aluminum layer with low hardness was
specimens fabricated by LPBF was examined through recip- easily worn at the beginning of the wear test, which resulted
rocating ball-on-disk wear tests on four specimens. These in the lower wear resistance of the specimen treated with AIH-
were the as-built material, a specimen subjected to LPBF and FPP at 1073 K.
then aged, and specimens processed using AIH-FPP at 723 or To investigate the wear behavior for each specimen, the
1073 K. Fig. 11 summarizes the wear loss for these samples wear tracks were analyzed using SEM and EDX. Fig. 13 pro-
and indicates that the loss for the LPBF þ aged specimen was vides SEM images and EDX maps of the wear track surfaces
lower than that for the as-built specimen. The metals sub- formed on each specimen. The wear track surfaces formed on
jected to AIH-FPP exhibited lower wear loss, while the loss for the specimens processed with AIH-FPP at 723 and 1073 K,
the 723 K sample was lower than that for the material treated which had layers of FeeAl intermetallic compounds, were
at 1073 K. found to contain Al. This indicates that the FeeAl interme-
Fig. 12 shows crossesectional profiles for wear tracks tallic compounds remained on the worn surfaces throughout
formed on these same specimens. The trend seen here is the wear tests, accounting for the improved wear resistance of
similar to the wear loss data in Fig. 11, meaning that the these materials after AIH-FPP. The SEM images also demon-
largest wear track was formed on the as-built specimen, and strate that the surfaces of the wear tracks formed on the AIH-
the tracks became smaller in the order of the LPBF þ aged, FPP-treated specimens were smoother than those formed on
AIH-FPP-treated at 1073 K and AIH-FPP-treated at 723 K the as-built and the LPBF þ aged specimens. This implies that
specimens. These results demonstrate that AIH-FPP using abrasive wear was suppressed on the surfaces of the AIH-FPP-
mechanically milled particles and the accompanying treated specimens, which also led to reduced wear loss.
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Fig. 12 e Crossesectional profiles of wear tracks formed on (a) as-built material, (b) LPBF þ aged specimen, and samples
processed with AIH-FPP at (c) 723 and (d) 1073 K.

Fig. 13 e SEM images and EDX maps for surfaces of wear tracks formed on as-built specimen, LPBF þ aged specimen and
specimens subjected to AIH-FPP at different temperatures.
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Fig. 14 e (a) SEM micrograph and (b) Fe and (c) Al maps of longitudinal cross-section of a fatigue specimen processed with
AIH-FPP at 723 K with peening time of 240 s.

3.3. Effect of AIH-FPP on fatigue properties of maraging fatigue specimens having the geometry shown in Fig. 2 were
steel specimens fabricated by LPBF processed using AIH-FPP while applying the thermal history
illustrated in Fig. 4(b). A temperature of 723 K was applied
The effect of AIH-FPP on the fatigue properties of the steel during AIH-FPP because this temperature had previously
specimen was assessed by performing axial fatigue tests using generated the best wear resistance. No heating time was
the as-built material, an LPBF þ aged specimen and samples employed after FPP to avoid the formation of voids in the
subjected to AIH-FPP. For comparison purposes, as-rolled and surface-modified layer, as indicated in Fig. 9. Fig. 14 shows an
rolled þ aged specimens were also tested. Prior to these trials, SEM micrograph and EDX maps of the longitudinal cross-
section of a fatigue specimen subjected to AIH-FPP at 723 K
with a peening time of 240 s. These images confirm that the
surface layer was similar to that formed on the disk-shaped
specimens (see Fig. 6). Moreover, an XRD analysis of the fa-
tigue specimen (data not included here) established that the
intermetallic compound Fe2Al5 formed on the surface of the
fatigue specimen, as was also the case for the disk-shaped
specimens.
Fig. 15 shows the results of the axial fatigue tests. The
specimens fabricated by LPBF (red data points) exhibit inferior
fatigue properties to those of specimens fabricated by rolling
(blue data points). The fatigue properties of both the as-built
material and the as-rolled specimen (circle) were improved
by aging (squares). When AIH-FPP was applied to the steel
samples fabricated by LPBF, the fatigue properties also
improved and approached those of the LPBF þ aged specimen.
Tsuchiya et al. [20] found that the bending fatigue limit of
additive-manufactured, solution-treated and polished mar-
aging steel was 460 MPa, while that laser-peened material was
640 MPa. Although the fatigue strength improvement effect of
AIH-FPP seems to be lower than that of laser-peening, the data
obtained in this study establish that AIH-FPP was able to
enhance the fatigue properties and wear resistance of LPBF-
processed maraging steel simultaneously and rapidly.
The results of the fatigue tests were further evaluated by
measuring the Vickers hardness, surface residual stress and
average surface roughness, Ra, for the fatigue specimens. The
results are summarized in Table 3.
The LPBF þ aged and rolled þ aged specimens exhibited a
higher Vickers hardness than the as-built and as-rolled
specimens. This indicates that aging increased the hardness
Fig. 15 e Axial fatigue test results for as-built material and of the steel irrespective of the manufacturing process, which
LPBF þ aged, AIH-FPP-treated, as-rolled and rolled þ aged would be expected to prevent fatigue crack initiation. This
specimens. explains the improved fatigue properties of the LPBF þ aged
384 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 1 : 3 7 3 e3 8 7

Table 3 e Vickers hardness, surface residual stress and average surface roughness data for fatigue specimens (mean ± SD).
Specimen Vickers hardness (n ¼ 20) Surface residual stress (n ¼ 4) Average surface roughness (n ¼ 10)

As-built 379.2 ± 7.4 HV 540 ± 162 MPa 0.045 ± 0.014 mm

LPBF þ aged 573.5 ± 13.3 HV 507 ± 126 MPa 0.048 ± 0.013 mm
AIH-FPP-treated 413.5 ± 7.4 HV 826 ± 180 MPa 1.703 ± 0.264 mm
As-rolled 311.6 ± 10.0 HV 357 ± 47 MPa 0.044 ± 0.015 mm
Rolled þ aged 552.1 ± 13.4 HV 390 ± 109 MPa 0.043 ± 0.008 mm

and rolled þ aged specimens. The hardness of the specimen the hardness of maraging steel depends on the aging time;
subjected to AIH-FPP was also increased relative to that of the thus, the short heating duration associated with the present
as-built specimen. A previous study [10] demonstrated that AIH-FPP processing resulted in some age hardening.

Fig. 16 e SEM images of fracture surfaces of (a) as-rolled and (b) rolled þ aged specimens.

Fig. 17 e SEM images and EDX maps of fracture surfaces of as-built specimen, LPBF þ aged specimen and specimen
processed using AIH-FPP.
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 1 : 3 7 3 e3 8 7 385

Fig. 18 e (a) Optical and (b) SEM micrographs along with (c) Fe, (d) Ti and (e) O maps of defect contained in as-built specimen.

The as-built and LPBF þ aged specimens exhibited similar roughness of the AIH-FPP-treated specimens did not affect
levels of surface compressive residual stress, while the as- their fatigue properties.
rolled and rolled þ aged samples also showed similar resid- The microstructure of an as-built specimen fabricated
ual stresses. These results are attributed to the identical using LPBF was analyzed by optical microscopy, SEM and EDX,
mirror-polishing process applied to all samples, which pro- and the results are shown in Fig. 18. The optical micrograph in
vided similar compressive residual stresses. However, the Fig. 18(a) shows the presence of several inclusions (appearing
AIH-FPP-treated specimen was found to have higher as dark regions), while the EDX maps indicate that the in-
compressive residual stress because the high-speed tool steel clusions contain Ti and O. Consequently, it appears that fa-
particles at the core of the milled particles introduced the tigue crack is initiated at inclusions comprising titanium
peening effect and inhibited the propagation of fatigue cracks. oxides. According to a previous study [41], the fatigue limit for
This is the reason for the improved fatigue properties of the materials manufactured by LPBF is correlated with the sizes of
AIH-FPP-treated specimen compared with the as-built spec- defects. Therefore, the fatigue properties of such metals could
imen. Although the residual stress distributions in the depth be enhanced by reducing the sizes of inclusions, such as by
direction for the various samples were not assessed in this improving the quality of the raw powder and optimizing the
study, FPP generally introduces compressive residual stress at processing conditions.
greater depths than mechanical polishing, thus providing
additional enhancement of the fatigue properties. When laser
peening was performed for maraging steel fabricated by LPBF, 4. Conclusions
a compressive residual stress of more than 1000 MPa was
introduced at the surface, which was higher than that intro- Maraging steel specimens fabricated by LPBF were subjected to
duced by AIH-FPP. This is assumed to be a reason why the AIH-FPP using mechanically milled particles to create layers of
fatigue strength improvement effect of AIH-FPP is lower than FeeAl intermetallic compounds and introduce a peening ef-
that of laser peening. fect. The surface properties of the treated steel were charac-
The surface roughness for the material subjected to AIH- terized, and wear and fatigue tests were performed to examine
FPP was higher than that for the other specimens, each of the effects of AIH-FPP on the wear resistance and fatigue
which was also polished to a mirror finish, because of colli- properties. The conclusions of the present study are as follows:
sions with the shot particles in the case of the former samples.
Fatigue cracks are often initiated at dents formed by the 1. AIH-FPP using mechanically milled particles can form
impact of these particles [39,40]; therefore, this increase in layers of FeeAl intermetallic compounds on the surfaces of
surface roughness could cause the fatigue properties of the maraging steel parts fabricated by LPBF, which is similar to
AIH-FPP-treated specimens to deteriorate. the case in which stainless steel is treated. This occurs
Although the surface characteristics of the specimens because Al is transferred from the shot particles to the
manufactured by LPBF were not inferior to those produced by specimen surfaces with a simultaneous combustion syn-
rolling, the fatigue properties of all the LPBF materials were thesis reaction. During AIH-FPP, the hardness of the sub-
inferior. The fracture surfaces of the failed specimens were strate also varies as a result of aging, although the
observed in an attempt to understand this outcome. Fig. 16 hardness (approximately 450HV) was lower than that
shows SEM images of the fracture surfaces of the as-rolled treated under the optimal aging condition reported in a
and rolled þ aged specimens. These images indicate that fa- previous study (approximately 600 HV).
tigue cracks were initiated at the surfaces of the specimens 2. The high hardness of these layers of FeeAl intermetallic
and propagated radially. Fig. 17 presents SEM images and EDX compounds improves the wear resistance of the maraging
maps obtained from crack initiation sites in the as-built, steel.
LPBF þ aged and AIH-FPP-treated specimens. In the case of 3. The fatigue properties of this material are also enhanced by
the specimens produced by LPBF, the fatigue cracks initiated AIH-FPP. This effect is attributed to the generation of
at the interior of the sample, and inclusions are apparent at compressive residual stress on the specimen surface together
the fatigue crack origin sites. According to the EDX maps with age hardening associated with heating during AIH-FPP.
shown in Fig. 17, Ti is present in the inclusions, so fatigue However, probably because of the lower compressive resid-
cracks initiated at these inclusions. This is the reason for the ual stress introduced at the surface of the AIH-FPP-treated
inferior fatigue properties. Because crack initiation occurred specimen, the fatigue strength improvement effect of AIH-
at the interior of each specimen, the greater surface FPP was lower than that of laser peening in a previous study.
386 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 1 : 3 7 3 e3 8 7

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Declaration of Competing Interest strength of EOS maraging steel produced by additive metal
machine. Fatig Fract Eng Mater Struct 2016;39:637e47.
https://doi.org/10.1111/ffe.12395.
The authors declare that they have no known competing
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financial interests or personal relationships that could have
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