Additive Manufacturing 29 (2019) 100803

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Ultra-high strength martensitic 420 stainless steel with high ductility T

a a b b c
Kamran Saeidi , Daniel Leon Zapata , Frantisek Lofaj , Lenka Kvetkova , Jon Olsen ,
⁎
Zhijian Shenc, Farid Akhtara,
a
Division of Materials Science, Luleå University of Technology, SE-97187 Luleå, Sweden
b
Institute of Materials Research of the Slovak Academy of Sciences, Watsonova 47, Košice, Slovakia
c
Department of Materials and Environmental Chemistry, Arrhenius Laboratory, Stockholm University, S-106 91 Stockholm, Sweden

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

Keywords: Martensitic 420 stainless steel was successfully fabricated by Selective laser melting (SLM) with > 99% relative
Selective laser melting density and high mechanical strength of 1670 MPa, yield strength of 600 MPa and elongation of 3.5%. X-ray
Tempering diffraction (XRD) and scanning electron microscopy disclosed that the microstructure of SLM 420 consisted of
Ultra-high strength colonies of 0.5–1 μm sized cells and submicron martensitic needles with 11 wt. % austenite. Tempering of as-
TRIP effect
built SLM 420 stainless steel at 400 °C resulted in ultra-high strength material with high ductility. Ultimate
Microstructure evolution
tensile strength of 1800 MPa and yield strength of 1400 MPa were recorded with an elongation of 25%. Phase
transformation analysis was carried out using Rietveld refinement of XRD data and electron backscattered dif-
fraction (EBSD), which showed the transformation of martensite to austenite, and resulted in austenite content of
36 wt. % in tempered SLM 420 stainless steel. Transformation induced plasticity (TRIP), austenite formation and
fine cellular substructure along with sub-micron martensite needles resulted in stainless steel with high tensile
strength and ductility. The advanced mechanical properties were compared with conventionally made ultra-
high-strength steels, and the microstructure-properties relationships were disclosed.

1. Introduction
Martensitic stainless steels are characterized by high strength and
hardness and are used in demanding applications like surgical instru-
ments, razor blades, bearings, etc. [1–3]. Undercooling can control the
amount of martensite formed in the steel microstructure and from
Koistinen–Marburger equation [4], the amount of martensite can be
predicted. Martensite has a body-centered tetragonal (BCT) crystal
structure, and since there are very few operable slip systems in BCT
structure, martensitic stainless steels are strong but brittle. Moreover,
the higher carbon content of martensite, which is all in solid solution,
promotes solid solution strengthening. To achieve an optimal combi-
nation of strength, hardness, and toughness further post-treatment such
as tempering is performed [5]. Using traditional manufacturing
methods for martensitic stainless steel, the resulting parts acquire
brittleness that makes it difficult to shape and machine the manu-
factured components.
Additive manufacturing (AM) has proven to be a promising way for
direct manufacturing of metallic parts with complex geometries and
functional structures [6–10]. Therefore, it is a promising technique to
produce components for applications within the automotive, aerospace
and medical industries [11–14]. The unique thermal regime occurring
during the SLM process can tune the chemistry, influence the me-
tallurgy, tailor the microstructure and improve the mechanical prop-
erties of fabricated materials. Saeidi et al. [15] observed significantly
improved mechanical properties of SLM 316 L austenitic stainless steel
that was caused by the hierarchical and fine microstructure of the 316 L
steel. Rashid et al. [16] verified that SLM manufacturing influenced the
metallurgical properties of 17-4 pH stainless steel. Hengbach et al. [17]
studied the phase transformation of, 900 °C, 1000 °C, and 1200 °C heat-
treated SLM duplex 2205 stainless steel, using EBSD technique and
reported the effect of phase content on the room temperature me-
chanical properties. Although many studies have been made on auste-
nitic and duplex stainless steels, only a few studies have been carried
out on martensitic stainless steels. Krakhmalev et al. [18] studied the
selective laser melting of duplex stainless steel powders and in-
vestigated the microstructure evolution during SLM, where they ob-
served partitioning and austenite reversion taking place owing to the
thermal cycling during SLM. Furthermore, they used numerical simu-
lation to explain the thermally activated processes during SLM. Xiao
Zhao et al. [19] investigated the hardness of SLM 420 material and
claimed it could meet the requirements for fabrication of plastic

⁎
Corresponding author.
E-mail address: farid.akhtar@ltu.se (F. Akhtar).

https://doi.org/10.1016/j.addma.2019.100803
Received 12 March 2019; Received in revised form 23 June 2019; Accepted 21 July 2019
Available online 24 July 2019
2214-8604/ © 2019 The Authors. 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/).
K. Saeidi, et al.
Fig. 1. SEM images of SLM 420 material, showing (a) cellular structure and martensite needles, (b) martensitic needles of submicron size inside the cells.
injection molding part with inner structural features. Jamshidinia et al.
[20] reported the development of core parameters for laser powder-bed
fusion (L-PBF) for 420 martensitic stainless steel and studied the effect
of processing parameters on the built properties of 420 stainless steel.
However, the effect of post-tempering of as-built SLM martensitic
stainless steel and its effect on the mechanical properties and evolution
of microstructure has not yet been studied and reported. This research
work focuses on the microstructure evolution and phase changes oc-
curring in tempered SLM martensitic stainless steel and reports the
development of an ultra-high strength martensitic stainless steel with
high ductility. The underlying mechanism causing superior mechanical
strength is explained and correlated to the microstructure.
2. Experimental
2.1. Powder precursors
The precursor material was gas-atomized spherical 420 stainless
steel powder granules (supplied by Sandvik Osprey Ltd, Neath, UK)
with a granular size of 20–53 μm. The overall chemical composition of
as-received powder provided by the manufacturer is 13 wt. % Cr,
0.8 wt. % Si, 0.8 wt. % Mn, 0.3 wt. % C and Fe balance.
2.2. Selective laser melting (SLM)
The SLM system was an EOS M270 ytterbium fiber laser with a
power of ˜200 W and a spot size of 70 μm (EOS Krailing, Germany).
Cubic samples and rods were built with dimensions 10 × 10 × 5 mm
and 40 × 4 × 1 mm, respectively. In order to obtain samples with the
satisfactory densification level, the laser power (P) was set at 195 W,
scanning speed (v) to 700 mm/s, layer thickness (h) and line spacing (s)
was set at 20 μm and 100 μm respectively, based on a series of pre-
liminary experiments. The applied laser volume energy density η was
defined by [20]. The laser volume energy density was calculated to be
139 J/mm3.
P 0.5–1 μm in size, and the martensite needles that are present in the cells
η= E . Q1
νsh
After separating the sample from the build plate, the density of the
SLM 420 sample was measured by the Archimedes method.
2.3. Post processing, tempering of as-built SLM 420
The tempering process was performed in a tube furnace
(Nabertherm, Germany) where the as-built SLM 420 samples were he-
ated to 400 °C with a heating rate of 300 °C/hr and held for 15 min and
cooled inside the furnace. The Ar atmosphere was used during heating
and cooling.
2.4. Phase analysis and microstructure observation
X-ray diffraction (XRD) measurements were conducted on a
Additive Manufacturing 29 (2019) 100803
Panalytical XPert diffractometer (Malvern Panalytical Ltd., UK) oper-
ating with a Copper X-ray tube in the angular range, 2θ, between 40°
and 100°. For microstructural analysis, samples were prepared using
standard techniques and etched in an acidic solution of 2% HF and 8%
HNO3. The microstructures of the etched samples were examined by a
Nikon optical microscope (ECLIPSE MA200, Tokyo, Japan) and scan-
ning electron microscope (SEM, JSM-7000 F, JEOL, Tokyo, Japan).
Preparation of the specimens for electron backscatter diffraction (EBSD)
started with systematically regular polishing and thereafter electro-
polishing the sample using a LectroPol-5 device (Struers, Ballerup,
Denmark) at 30 V for 5 s. The EBSD was performed by (JSM-IT300)
equipped with Oxford NordlysMax3 system under the acceleration
voltage of 20 kV; tilt angle 70°; step size 150 nm. Data were post-pro-
cessed by HKL Channel 5 software, and Image processing was done by
the Tango software.
2.5. Mechanical properties and microhardness
For the tensile test, dog-bone-shaped samples were cut by an
electro-spark machine from two bulk bars. The length of the reduced
section on the samples was 30 mm, and the gauge length between the
gauge marks as well as tensometer contacts was 25 mm. The tensile
tests were performed on an upgraded Tiratest 2000 testing machine
with the crosshead speed of 0.5 mm/min. Microhardness measurements
were carried out using a Zwick/ Roell ZHV indenter under a load of
1 kgf with a dwell time of 10 s. The microhardness reported were the
average of ten indents from different locations.
3. Results and discussion
The relative density of the as-built SLM 420 stainless steel was
measured to be 99.8% by the Archimedes method. The scanning elec-
tron micrographs of as-built SLM 420 in Fig. 1(a) shows a cellular mi-
crostructure with martensite needles in random orientation. The higher
magnification micrograph in Fig. 1(b) shows that the cells are of
are of submicron size. The microstructure of SLM 420 in current work
(1)
shows martensite needles similar to reported by Krakhmalev et al. [18].
These needles, however, are much smaller than the martensitic needles
formed by quench and partitioning treatment reported in the literature
[21,22] with size in tens of microns. Randomly oriented martensite
needles and variability of the size of the cells (Fig. 1b) indicate the
complex and heterogeneous microstructure of as-built SLM 420. The
heterogeneity is due to the considerably high cooling rate (105–107 K/s)
of the melt pool, high and asymmetrical temperature gradients and
overlapping of the scanning tracks during the SLM process [23].
XRD diffractogram of the as-built SLM 420 is shown in Fig. 2.
Martensite and austenite diffraction peaks are detected. Rietveld re-
finement and quantitative phase analysis measured the austenite con-
tent of approximately 10 wt. % and the balance was martensite. The
XRD diffractogram did not show the presence of secondary carbide.
Hongyu Chen et al. [24] reported that rapid solidification in SLM
2
K. Saeidi, et al. Additive Manufacturing 29 (2019) 100803

Fig. 2. XRD diffractogram of SLM 420 stainless steel showing martensite and
austenite phases.
Fig. 3. Stress-strain curve obtained at room temperature from as-built and
tempered SLM 420 stainless steel.
process did not offer sufficient time for diffusion of alloying elements
and formation of carbides, allowing the carbide formers to remain in
the solid solution with iron.
Fig. 3 shows room temperature tensile test curve for the as-built
SLM 420 material, where the material deforms elastically with a yield
strength of approximately 600 MPa then deforms plastically with-
standing a tensile stress of 1670 MPa and 3.5% of elongation before
failure.
The mechanical properties of as-built SLM 420 are listed in Table1
along with the mechanical properties of martensitic stainless steels from
the literature for making a comparison. It can be seen that the tensile
strength of 1670 MPa of the SLM 420, in current work, is superior to the
conventional 420 material, with 800 MPa [25]. The increase in the
mechanical strength of selective laser melted for other alloys such as
titanium has been reported in the literature [26] Not only the me-
chanical properties but also the microhardness of as-built SLM
420,650 HV, is higher than conventional 420 materials. Although the
mechanical strength is exceeding the strength of conventional AISI 420,
the ductility is much lower which limits the applications for the SLM
420.
After tempering heat treatment at 400 °C for 15 min, the mechanical
properties of SLM 420 were evaluated. As seen from the room tem-
perature tensile test curves of heat treated SLM 420 in Fig. 3, a tensile
strength of 1800 MPa and two times higher yield strength of 1400 MPa
is obtained as compared to as-built SLM 420. The mechanical strength
is higher than ultra-high strength stainless steel, as it is exceeding
1750 MPa [27]. Moreover, it can be seen in Fig. 3 that the ductility of
the heat treated SLM 420 has increased five times (total elongation of
25%) than as-built SLM 420.
The mechanical properties of the tempered SLM 420 material along
with data from literature of ultra-high strength steels is listed in
Table 1. As seen from the table that the mechanical properties and
ductility of the heat treated SLM 420, obtained in this work, are su-
perior than ultra-high strength steel sheets (UHSS) produced by ther-
momechanical controlled processing (TMCP) and cold rolling/air
cooled (CR + AC) sheets, as reported by Chen et al. [28]. It has been
reported that ultra-high strength was obtained in steels via extensive
plastic deformation, hot working or thermomechanical treatment, and
the processing requires extensive energy. In comparison, the ultra-high
strength SLM 420 stainless steel has been obtained by a facile and low-
cost heat treatment process after SLM. Fig. 4 shows the fracture surfaces
of as-built SLM 420 and tempered 420 stainless steel. The fracture
surface of as built SLM 420 in Fig. 4(a) shows no indication of ductile
mode of fracture, whereas the tempered SLM 420 clearly shows dimples
representing the ductile mode of fracture, Fig. 4(b). This verifies the
observed low elongation to failure of 3.5% for the as-built SLM 420 as
compared to 25% for the tempered SLM 420 (see Fig. 3).
The higher ductility and strength of the heat treated SLM 420 sug-
gests that the microstructure and phases have been changed on heat
treatment at 400 ◦C for 15 min. The microscopy and X-ray diffraction
analysis was performed to understand the mechanism of enhancement
in the mechanical properties.
The XRD diffractogram in Fig.5 (a) shows that the heat treated SLM
420 material consists of martensite and austenite. No other XRD peaks
from secondary carbides are detectable. Quantitative phase analysis of
Rietveld refined XRD data measured the amount of austenite in the
tempered SLM 420 around 36 wt %. Fig. 5(b–c) shows the inverse pole
figure (IPF) and EBSD phase mapping, respectively. As seen from the
phase mapping, the amount of austenite is considerable; which is ap-
proximated to 30 wt. %, confirming the results of the quantitative phase
analysis using XRD. Moreover, the small fraction of carbide phases in
the microstructure was detected. The absence of carbide XRD diffrac-
tion peaks might be related to the small size and small content of the
carbides. The carbides are distributed homogenously with no specific
segregation site. The IPF in Fig. 5(b) shows the small size of the grains
and microconstituents with random orientations and absence of texture.
The increase in the austenite phase content can be explained by the
austenite reversion due to the carbon partitioning process that occurs
during tempering [29,30]. Upon quenching, the microstructure consists
of retained FCC austenite and BCT martensite. The trapped carbon in
the martensite results in the distortion of the crystal structure of mar-
tensite and introduces stresses. During tempering, carbon partitions
from the supersaturated martensite to the retained austenite, resulting
in a stabilization of austenite. In Fe-Cr-C system, the carbon partitioning
temperature is low, which results in stagnation of carbon atoms at the

Table 1
Mechanical properties of the SLM 420 material post tempered 420. Data from literature have been added for comparison.
Type of material Tensile strength Yield strength Elongation Microhardness (HV)
(MPa) (MPa) (%)

SLM 420 (this work) 1670 ± 54 600 ± 5 3.5 ± 0.3 650 ± 15

Annealed cold drawn AIS 420 [25] 800 700 6-7 —
SLM 420 [22] Not measured Not measured Not measured 450-500
Post tempered 420 (this work) 1800 ± 7 1400 ± 12 25 ± 0.6 500 ± 10
UHSS (CR + AC) [28] 1550 1032 13.7 486
UHSS (TMCP) [28] 1545 1020 11.9 532

3
K. Saeidi, et al. Additive Manufacturing 29 (2019) 100803

Fig. 4. Fracture surface of a) as-built SLM 420 and b) tempered SLM 420 at 400 ◦C for 15 min.

martensite-austenite interface due to the higher diffusion rate of carbon

in BCC than in FCC iron. The carbon-rich interfaces act as nucleation
sites for the reversion of austenite due to the high local driving force for
austenite reversion provided by the carbon [30]. The competition of
carbon could be the plausible mechanism of the reversion of austenite
during the heat treatment at 400 °C. Fig. 6. shows the XRD diffracto-
gram from the fracture site of the tensile sample tempered at 400 °C and
comparison with sample tempered at 400 °C before the tensile test.
As seen the austenite content measured by Rietveld refinement for
the fracture site of the tensile sample has been reduced to 14 wt.%,
implying that the austenite has been transformed to martensite upon
loading and deformation. The phenomenon is regarded as a transfor-
mation induced plasticity (TRIP). During the TRIP effect, the retained
austenite phase is transformed to martensite. Thus, the increase in the
strength happens by strain hardening (Fig. 4). The TRIP effect allows
for the observed enhanced strength and ductility [31]. The TRIP effect
is seen in TRIP steels where the steels possess a microstructure con-
sisting of austenite with sufficient thermodynamic instability such that
Fig. 6. XRD diffractogram from the fracture site of tensile sample tempered at
the phase transformation of austenite to martensite is obtained during
400 °C and comparison with sample tempered at 400 °C before tensile testing.
the plastic deformation. TRIP phenomenon has been previously re- The austenite content has been reduced from 36.5 to 14 vol. %.
ported in carbon steels produced by selective laser melting [32] and
high Manganese steels [33].

Fig. 5. a) XRD diffractogram of SLM 420 tem-

pered at 400 °C for 15 min, showing the co-
existence of martensite and austenite, b) IPF
representing the random orientation of the
grains and fine microstructure, c) EBSD phase
mapping revealing the existence of large vo-
lume fraction of austenite in the tempered SLM
420 material.

4
K. Saeidi, et al.
Fig. 7. (a–b) SEM image of post tempered SLM 420 showing cell colonies and coarse martensite needles.
Fig. 7. Shows SEM images of the post tempered SLM 420. As seen,
the overall microstructure is similar to as-built SLM 420 (Fig.1) with
cell colonies and martensite needles and the microstructure keeps its
fine cellular structure, shown in Fig. 5(b). However, the martensite
needles are relatively coarser compared to as-built SLM 420. It is
therefore concluded that the combination of fine microstructure, higher
content of austenite, coarser martensite needles and TRIP phenomenon
have contributed to the high strength and ductility of the post tempered
SLM 420 categorizing it as an ultra-high strength steel.
4. Conclusion
The conclusions are as follows
1 The 420 stainless steel parts fabricated by SLM were fully dense with
˜99.8% relative density and were characterized by ultrafine and
heterogeneous microstructure, containing colonies of cells with the
size between 0.5–1 μm and martensitic needles in submicron scale.
2 The as-built SLM 420 consisted of austenite and martensite phases
with 11 wt. % austenite and depicted a high tensile strength of
1670 MPa and elongation of 3.5%.
3 The SLM 420 specimen heat-treated at 400 °C exhibited a high
fraction of austenite, around 36 wt. %, which was much higher than
as-built SLM 420.
4 The heat treated SLM 420 exhibited a very high tensile strength of
1800 MPa and yield strength of 1400 MPa and showed five times
higher ductility, 25% elongation, compared to as-built SLM 420.
5 The TRIP effect caused by the heat treatment of the SLM 420 at
400 °C improved the mechanical strength and ductility of the heat
treated SLM 420.
6 The heat treated SLM 420 stainless is categorized as an ultra-high
strength stainless steel.
Acknowledgment
Authors acknowledge the funding support from Carl Tryggers
foundation (grant. No. CTS 16:6) and Swedish Foundation for Strategic
Research (SSF) for infrastructure fellowship grant (RIF14-0083) for
current research.
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