Journal of Alloys and Compounds 785 (2019) 305e311

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Journal of Alloys and Compounds

journal homepage: http://www.elsevier.com/locate/jalcom

Nitrogen doped Co-Cr-Mo-W based alloys fabricated by selective laser

melting with enhanced strength and good ductility
Bo Wang a, Xinglong An a, Zonglian Huang a, Min Song a, Song Ni a, Shaojun Liu a, b, *
a
State Key Laboratory for Powder Metallurgy, Central South University, Changsha, 410083, China
b
Shenzhen Research Institute, Central South University, Shenzhen, 510085, China

a r t i c l e i n f o a b s t r a c t

Article history: Nitrogen doped Co-Cr-Mo-W based alloys with substantially enhanced strength and good ductility were
Received 24 October 2018 successfully fabricated by selective laser melting (SLM). The results showed that nitrogen suppressed the
Received in revised form formation of hexagonal close packed (hcp) ε phase martensitic through hindering the Shockley partial
29 December 2018
dislocations slip. Combining with SLM, doping nitrogen into Co-Cr-Mo-W alloys provides an effective
Accepted 14 January 2019
Available online 17 January 2019
strategy to significantly improve the strength and maintain the ductility simultaneously. The yield
strength, ultimate tensile strength and elongation of 0.086 (wt.%) N-doped Co-26Cr-5Mo-5W alloys are
~1027 MPa, ~1295 MPa and ~18.2%, respectively.
Keywords:
Co-Cr-Mo-W alloy
© 2019 Elsevier B.V. All rights reserved.
Selective laser melting
Nitrogen addition
Martensitic transformation
Mechanical properties

1. Introduction nano-scaled Cr2N precipitates or short-range ordering (SRO) that

In addition to good ductility, high strength of CoeCreMo alloys
is of crucial importance to the improved durability of their appli-
cations in total hip and knee replacements, orthopedic implant,
dental crowns and replaceable dentures [1e4]. It has been shown
that grains size, precipitates along the grain boundaries, volume
fraction of g and ε phases, dislocations and stacking faults signifi-
cantly influence the mechanical properties of Co-Cr-Mo alloys
[5e7].
It is well known that as-cast Co-Cr based alloys usually contain
casting defects such as shrinkage porosity, coarse dentritic struc-
ture and carbide precipitates that severely deteriorate the ductility
of the alloys [2,8e12]. Previous studies have shown that Ni can
significantly enhance the ductility of the as-cast Co-Cr alloys due to
the inhibition of martensitic transformation from face-centered
cubic (fcc) structured g phase to hexagonal close packed (hcp)
structured ε phase [13e16]. Unfortunately, Ni can cause allergies
and cancer in living organisms. Further investigations revealed that
doping nitrogen can improve the ductility of biomedical Co-Cr al-
loys as well [17,18]. Small amount of nitrogen addition can induce
* Corresponding author. State Key Laboratory for Powder Metallurgy, Central
South University, Changsha, 410083, China.
E-mail address: liumatthew@csu.edu.cn (S. Liu).
inhibit the dislocation slip, thereby suppressing the martensitic
transformation from g phase to ε phase [19e22].
Selective laser melting (SLM) is considered as one of the
advanced metal additive manufacturing (AM) technologies appli-
cable to the complex geometry components [23e26]. Compared to
that of the traditionally manufactured alloys, rapid cooling and
large temperature gradients of the alloys during the SLM processing
can result in a significant difference in the microstructure of Co-Cr-
Mo alloys. Owing to the high demand for personalized custom-
ization for patients, more attention has been paid to the selective
laser melting (SLM) of Co-Cr based alloys [27e31]. However, a
fundamental understanding of the relationship between the pro-
cessing, microstructure, martensite phase transformation, and
mechanical properties in SLM-ed Co-Cr-Mo alloys is still lacking.
Especially, there are very few reports on the structure, mechanical
properties and martensitic transformation of N-doped Co-Cr alloys
fabricated by SLM until now. It is believed that the main reason is
that it is difficult to dope nitrogen into the Co-Cr alloys powders
during the powder gas atomization fabrication [32].
In the present study, nitrogen doped biomedical Co-26Cr-5Mo-
5W based alloy with significantly enhanced strength and good
ductility was successfully fabricated by selective laser melting.
Especial attention was paid on the relationship between SLM
induced microstructure, martensitic transformation, and

https://doi.org/10.1016/j.jallcom.2019.01.178
0925-8388/© 2019 Elsevier B.V. All rights reserved.
306 B. Wang et al. / Journal of Alloys and Compounds 785 (2019) 305e311

mechanical properties of N-doped Co-Cr-Mo-W alloys. Table 1

Chemical compositions of Co-Cr-Mo-W alloys (wt.%).

Alloy Co Cr Mo W N Si Mn C
2. Materials and methods
N-free Bal. 25.46 5.04 5.51 0.018 1.86 0.72 0.012
Nitrogen free and nitrogen doped Co-Cr-Mo-W alloy powders N-doped Bal. 25.67 4.98 5.08 0.086 1.70 0.77 0.019

were prepared by gas atomization in nitrogen atmosphere. Cr2N

powder was used as the nitrogen source. It should be noted that
Cr2N powder is easily decomposed during the gas atomization
processing. Therefore, it is difficult to dope high nitrogen content
into Co-Cr-Mo-W alloy powder [32]. The particle size was measured
by laser particle size analyzer (Mastersizer). Fig. 1 (a) and (b) shows
the powders are of a well spherical shape containing some satellites
and very few holes in both N-free and N-doped alloys. As shown in
Fig. 1(c), the N-free alloy powder for SLM process has a particle size
distribution ranging from ~16.5 to ~49.0 mm and an average size of
~29.0 mm. However, N-doped powder has a particle size ranging
from ~16.6 to ~52.3 mm and an average size of ~29.3 mm (see
Fig. 1(d)), respectively. The chemical compositions of the alloy
powders evaluated by an inductively coupled plasma optical
emission spectrometer (ICP-OES) are listed in Table 1. It can be seen
that the N-containing alloy has a nitrogen content of 0.086 wt%.
The samples fabricated by SLM are controlled by four main
processing parameters: laser power (P), hatch spacing (h), scanning
speed (v), and layer thickness (t). During SLM, the scanning direc-
tion of the sample is kept 67
angle rotation for the two consecutive
layers in argon atmosphere. These factors determine the energy
supplied by the laser beam to a unit volume of powder material,
described as volumetric energy density (VED), which is defined as
follows:
P
VED ¼
vht
The parameters used for preparing the samples were: laser
power of 160e190 W, hatch spacing of 0.07e0.09 mm, scanning
speed of 400e600 mm/s and layer thickness of 0.03 mm. Tensile
specimens and cubic samples with a dimension of 10  10  10 mm
were prepared by SLM equipment (Farsoon FS271M) for mechani-
cal testing and microstructural characterization, respectively.
The tensile tests of the specimens were performed by MST
Alliance RT machine (MTS systems, Eden Prairie, MN) with a testing
speed of 1.67  105 m/s at room temperature. The crystal structure
of SLM-ed alloys is determined by X-ray diffraction (XRD; D/
max2550pc) with Cu-Ka radiation (k ¼ 0.154 nm). The microstruc-
tures of SLM-ed Co-Cr-Mo-W alloys were characterized by scanning
electron microscopy (SEM; Model Quanta 250 FEG), electron
backscattered diffraction (EBSD; Helios NanoLab G3 UC, FEI Czech
Republic) and transmission electron microscopy (TEM; Titan G2
FEI) operated at 20 kV, 18 kV and 200 kV, respectively. The samples
for XRD were mechanically grinding and subsequently polished
using 0.2 mm colloidal silica solution and were then mirror polished
using 0.05 mm colloidal silica solution. The samples for SEM char-
acterization were further corroded by etching solution (HCl:
H2O2 ¼ 9: 1). The samples for EBSD were prepared using electro-
lytic double spray thinning (Tenupol-5, DNK). The samples for TEM
were prepared by sandpaper grinding to 30 mm and electrolytic
double spray thinning (Tenupol-5, DNK) or subsequent ion milling
(Gatan 691, USA).
3. Results and discussion
For comparison purpose, the performance of Co-Cr based alloys
(1) fabricated by casting and SLM processing from different sources is
summarized in Fig. 2. The same color and logo represents the
properties of Co-Cr alloys studied by a scholar, including ultimate
tensile strength (UTS, upper) and yield strength (YS, lower). The
black circles in Fig. 2 shows the results of N-free and 0.086 (wt.%) N-
doped Co-26Cr-5Mo-5W alloys in the present investigation, which
were fabricated by SLM with laser energy density of 190.5 J/mm3. It
is clear that the alloys present well-balanced strength and ductility.

Fig. 1. Powder morphology of (a) N-free and (b) N-doped Co-Cr-Mo-W alloy, corresponding to the particle size distribution of (c) N-free and (d) N-doped Co-Cr-Mo-W alloy.
 B. Wang et al. / Journal of Alloys and Compounds 785 (2019) 305e311
Fig. 2. The performance of Co-Cr based alloys fabricated by casting and SLM pro-
cessing from different sources.
It can be seen that doping nitrogen significantly increases the ul-
timate tensile strength and maintains the fracture elongation. The
maximum elongation and ultimate tensile strength are ~18.2% and
~1295 MPa, respectively. Especially, the yield strength of the alloys
increases by 18% (~1027 MPa), compared to that of nitrogen free
alloys. These results clearly demonstrate that combining with SLM,
doping nitrogen into Co-Cr-Mo-W alloys provides an effective
strategy to significantly improve the strength and maintain the
ductility.
The fracture surface morphologies of N-free and N-doped Co-Cr-
Mo alloys after tensile tests are shown in Fig. 3(aed). The high
magnification images of the red square regions in Fig. 3(a) and (c)
Fig. 3. SEM images of fracture morphology: (a, b) N-free and (c, d) N-doped Co-Cr-Mo-W alloy.
307
are shown in Fig. 3(b) and (d), respectively. Obvious necking
behavior is not observed during mechanical testing. Under low
magnification, fault steps are observed in Fig. 3(a) and (c), which is
packed with cleavage surfaces (black arrows) and torn edges sur-
rounding the planes. Moreover, wedge-type cracks (white arrows)
are also observed in Fig. 3(a) and (c). The fracture of this nature is
considered to be a typical brittle fracture characteristic. The
dimple-like patterns in Fig. 3(b) and (d) are observed, derived from
the cellular dendrites. The dimples seem to be uniform with a size
of <1 mm. This characteristic of under high magnification repre-
sents a ductile fracture mode. The fracture surfaces of N-free and N-
doped Co-Cr-Mo-W alloys in Fig. 3 have obvious dimples and
cleavage steps, so the fracture modes of both are recognized as
quasi-cleavage fracture. This quasi-cleavage-type fracture is most
probably due to internal stresses and local thermal effects induced
by selective laser melting.
It is well known that fcc g phase of Co-Cr based alloys is more
stable at high temperature. In contrast, hcp ε phase is the equilib-
rium phase at room temperature. It has been shown that nitrogen
can be used to effectively improve the ductility of Co-Cr based al-
loys by suppressing g/ε martensitic transformation [7,20,33e36].
Fig. 4(aec) shows the XRD patterns for N-free and N-doped Co-Cr-
Mo-W powders and alloys, respectively. Fig. 4(a) shows that only g
phase is observable in both N-free and N-doped powder. In
contrast, Fig. 4(b and c) shows that g phase and ε phase co-exist in
N free and N-doped Co-Cr-Mo-W alloys after SLM. Moreover, it is
clear from Fig. 4(b and c) that the relative intensity of the (200)g
and (220)g diffraction peaks of the N-doped alloys increases,
compared to that of the N-free SLM-ed alloys. Meanwhile, the in-
tensity of the (1011)ε and (1010)ε peak decreases. Fig. 4(d) shows
that the hcp ε content of the N-doped alloys significantly decreases
from 34.8% for the N-free Co-Cr-Mo-W alloy to 3.04%. These results
show that nitrogen can effectively suppress g / ε martensitic
transformation of SLM-ed Co-Cr-Mo based alloys.
308 B. Wang et al. / Journal of Alloys and Compounds 785 (2019) 305e311

Fig. 4. (a) Powder XRD results of Co-Cr-Mo-W alloy. (b) XRD results of SLM-ed N-free and N-doped Co-Cr-Mo-W alloy at the same laser energy density.

Typical cross-sectional SEM images of N-free and N-doped Co-
Cr-Mo-W alloys by SLM are shown in Fig. 5. As shown in Fig. 5(a)
and (c), both N-free and N-doped Co-Cr-Mo-W alloys by SLM pre-
sent a unique microstructure containing a large number of fusion
boundaries, solidification cellular structures. Especially, both SEM
images of N-free and N-doped alloys in Fig. 5(b) and (d) show dense
structure with few casting defects, such as shrinkage porosity,
coarse dentritic structure and carbide precipitates that can signif-
icantly deteriorate the ductility of the materials. The structures of
N-free and N-doped alloys are composed of equiaxed and elongated
grains as well. The diameter and height of the elongated grain
structure is estimated to be ~0.2 mm and ~10 mm, respectively.
Additionally, the walls between the solidification cellular are much
brighter than the intergranular boundaries. This unique micro-
structure of as-built Co-based alloys is believed to be mainly due to
high localized melting, large temperature gradient, and fast
solidification rate during the SLM processes.
To further observe the texture of the grains, the EBSD charac-
terization of N-free and N-doped Co-Cr-Mo-W alloy from cross-
sectional view is provided in Fig. 6. Fig. 6(a) and (b) shows the in-
verse pole figure (IPF) of the as-SLMed N-free and N-doped alloys,
respectively. The elongated and fine grain morphology is visible in
the side view, where red color grains have a 〈001〉 orientation
parallel to the building direction. Since the samples preparation
process by SLM are of large temperature gradients and fast solidi-
fication rate, there are two elongated and fine grain portions cor-
responding to SEM images in Fig. 5. These elongated grains in the
cross-sectional view of Fig. 6(a) and (b) are typically solidified along
the weld pools and blocked between the weld pools. Subsequently,
fresh fine grains with random crystal orientation are formed, which
result in more grain orientations. It is noticeable that N-free alloys
have a 〈001〉 orientation and more red color areas in N-free alloys

Fig. 5. SEM images showing typical surface morphologies of SLM processed of (a, b) N-free and (c, d) N-doped Co-Cr-Mo-W alloys.
 B. Wang et al. / Journal of Alloys and Compounds 785 (2019) 305e311
Fig. 6. EBSD maps of as-SLM (a, c) N-free and (b, d) N-doped Co-Cr-Mo-W alloys: (a, b) inverse pole figure (IPF), (b, d) boundary maps.
(see Fig. 6(a) can be observed than in N-doped alloys (see Fig. 6(b)).
Fig. 6(c) and (d) shows the distribution of grain boundary map, in
which the black lines represent the high angle boundaries (HABs)
with misorientation angles greater than 15
. The green lines and
red lines represent the low angle boundaries (LABs) with misori-
entation angle in the range of 2e15
and annealing twin boundaries
(ATBs), respectively. Obviously, the regions of elongated and fine
grains of N-free alloy have plentiful LABs in Fig. 6(c), while the fine
grain areas of N-doped alloy is more than that of the elongated
grain areas to LABs in Fig. 6(d). The appearance of ATBs in both
alloys may be caused by the remelting of the upper layer of powder
during the laser sintering the subsequent layer, which is equivalent
to the annealing process.
Fig. 7(a and b) and Fig. 7(c and d) show the bright-field TEM
images of the N-free and N-doped alloys, respectively. The stacking
faults (SFs) and precipitates are marked by black and blue arrows,
respectively. Two directions of the SFs with a 70.5
angle were
observed in both N-free and N-doped alloys, as shown in Fig. 7(a)
and (c). Fig. 7(b) shows a large ε lamella (~100 nm in width). The
inserted images in Fig. 7(b) show the corresponding selected area
electron diffraction (SAED) pattern of the red circled area and the
FFT-filtered HRTEM image of the blue rectangular area in N-free
alloy along ½110 direction. It can be seen from SAED patterns in
309
Fig. 7(b), the orientation relation between the fcc g phase (red line)
and hcp ε phase (yellow line) obeys the Shoji-Nishiyama rule [37]
that can be described as: {111}g//{0001}ε and 〈110〉g//〈1120〉ε. It
can be clearly seen that the stacking sequence was changed from
FCC phase: … ABCABC … to HCP phase: … ABABAB …. Fig. 7(c) and
(d) show that no obvious ε phase but some thin SFs and precipitates
can be found in N-doped Co-Cr-Mo-W alloys. These results indi-
cated that both the size and amount of ε phase in N-free alloys are
larger than those in N-doped alloys, which are consistent with the
XRD results shown in Fig. 4.
The SFs can be easily formed in our study due to the low stacking
fault energy of Co-Cr based alloys, in which the stacking fault en-
ergy can even be negative at room temperature [14,21,34,38]. It is
well-known that SFs can be regarded as local ε-layers pinning in the
fcc g matrix [21]. It is reported that the formation of thin ε-layer is
caused by three different types of Shockley partial dislocations with
different shear directions 〈112〉 periodically gliding on every second
{111} planes to release the local strain [39]. The stacking sequence
in [111]g planes has been changed from ABCABC … to ABABAB ….
Then, some new ε-layers nucleate closely to the preexisting ones
and finally grow together. Eventually, the large ε-phase can be
formed, as shown in Fig. 7(b). The results indicate that N doping has
a significant influence in suppressing martensitic transformation by
310 B. Wang et al. / Journal of Alloys and Compounds 785 (2019) 305e311
Fig. 7. Bright-field TEM images of (a, b) N-free and (c, d) N-doped Co-Cr-Mo-W alloys through selective laser melting (SLM).
inhibiting Shockley partial dislocation slip since the dislocation slip
is a key step to nucleate ε phase. Furthermore, previous studies
revealed that short-range ordering (SRO) or nanoscale Cr2N pre-
cipitates can be generated in the g matrix in N-doped Co-Cr-Mo
alloys, which act as obstacles for Shockley partial dislocations
gliding and subsequently increase the energy barrier for g/ε
martensitic transformation [20,33].
In this investigation, no obvious SRO and Cr2N precipitates were
found, but some precipitates were observed in the black arrows in
Fig. 7(a) and (c). The pinning role of the precipitates could be
another reason for inhibiting the g/ε martensitic transformation.
It should be mentioned that further investigation is necessary to
clarify the martensitic transformation of Co-Cr based alloys during
SLM processing.
Recently, a method has been proposed to strengthen the cast Co-
Cr alloys by increasing Cr and N contents [21]. It was reported that
increasing the Cr content results in the increase of nitrogen solu-
bility in Co-Cr alloys. Consequently, the fcc g phase in
Coe33Cre5Moe0.3N (wt.%) alloys can be stabilized at room tem-
perature, resulting in significantly improved strength and ductility.
Additionally, tungsten can also be used to stabilize the g-phase [40].
It is stressed that the solubility of nitrogen in Co-Cr alloy powder is
still limited (0.086 wt%) in the present investigation. It is thus ex-
pected that the strength and ductility of the CoeCr alloys by SLM
could be further enhanced by adjusting the composition of Cr, W,
and N in CoeCreW-based alloys. Especially, personalize low-profile
spinal-system devices with a reduced rod diameter may potentially
be realized with extremely high strength and good ductility of
CoeCreMo alloys.
4. Conclusion
Combining with SLM, doping nitrogen into Co-Cr-Mo-W alloys
provides an effective strategy to significantly improve the strength
and maintain the ductility. The major results are summarized
below:
(1) The mechanical properties of N-free and N-doped Co-Cr-Mo-
W alloy is better than that of traditional casting alloys. After
doping 0.086 (wt. %) nitrogen Co-Cr-Mo-W alloy, the yield
strength, the ultimate tensile strength, and the elongation of
the alloy can reach ~1027 MPa, ~1295 MPa, and ~18.2%,
respectively.
(2) In the N-doped alloy, the content of hcp ε phase was signif-
icantly reduced from 34.8% in N-free alloy to 3.04%. Doping
nitrogen, which effectively suppresses the fcc g phase to hcp
ε phase martensitic transformation, significantly increases
the yield strength and maintains the fracture elongation.
(3) The fracture surfaces of N-free and N-doped Co-Cr-Mo-W
alloys have obvious dimples and cleavage steps, so the frac-
ture modes of both are recognized as quasi-cleavage fracture.
(4) N-free Co-Cr-Mo-W alloys have more 〈001〉 orientation can
be observed than the N-doped alloys. Both N-free and N-
doped Co-Cr-Mo-W alloys contain a large number of low
angle boundaries (LABs) and a few annealing twin bound-
aries (ATBs).
(5) The structures of N-free and N-doped alloys are composed of
equiaxed and elongated grains as well. The diameter and
height of the elongated grain structure is estimated to be
~0.2 mm and ~10 mm, respectively.
 B. Wang et al. / Journal of Alloys and Compounds 785 (2019) 305e311
Data availability
The raw/processed data required to reproduce these findings
cannot be shared at this time due to technical or time limitations.
However, the raw/processed data can be provided as request.
Acknowledgement
The utilities of facilities in State Key Laboratory for Powder
Metallurgy and Institute for Materials Microstructure at Central
South University are sincerely acknowledged. This work was
financial supported by Shenzhen Technical Innovation and Tackling
Program (Grant Nos. 20170410221235842).
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