Corrosion Science 161 (2019) 108189

Contents lists available at ScienceDirect

Corrosion Science
journal homepage: www.elsevier.com/locate/corsci

Short Communication

On the unusual intergranular corrosion resistance of 316L stainless steel T

additively manufactured by selective laser melting
Majid Laleha,b, Anthony E. Hughesb,c, Wei Xua, Nima Haghdadib, Ke Wangb, Pavel Cizekb,
Ian Gibsona, Mike Yongjun Tana,b,
⁎

a
Deakin University, School of Engineering, Faculty of Science and Technology, Geelong Waurn Ponds Campus, Waurn Ponds, Victoria, 3216, Australia
b
Deakin University, Institute for Frontier Materials, Geelong Waurn Ponds Campus, Waurn Ponds, Victoria, 3216, Australia
c
Commonwealth Scientific and Industrial Research Organisation (CSIRO), Mineral Resources, Private Bag 10, Clayton South, Victoria, 3169, Australia

ARTICLE INFO ABSTRACT

Keywords: The intergranular corrosion (IGC) resistance of 316L stainless steel (316L SS) produced by selective laser melting
Intergranular corrosion (SLM) was investigated using microscopy analysis and electrochemical measurements. The IGC resistance of
316L stainless steel SLM-produced 316L SS, determined using a double-loop electrochemical potentiokinetic reactivation test, was
Additive manufacturing found to be substantially higher than that of conventional 316L SS. This unusual behaviour was explained by the
Grain boundary
fact that no Cr-rich precipitates were detected for SLM-produced specimens after long-term sensitisation heat-
Precipitation
treatment and those SLM-produced specimens exhibited a high frequency of twin boundaries and low-angle
grain boundaries along with fine grains, leading to the avoidance of localised Cr depletion.

1. Introduction properties such as weaker erosion-corrosion resistance of SLM-pro-

Austenitic stainless steels are widely used in engineering structures
operating at elevated temperatures such as in steam generating plants
as piping and superheating tube materials. Under such harsh environ-
mental conditions, intergranular corrosion (IGC) of conventional
stainless steels is frequently observed, especially in sections joined by
welding at temperatures between 500 and 850 °C. Additive manu-
facturing (AM), an emerging net-shape layer-wise fabrication process, is
being adopted for producing structural components used at elevated
temperatures because of its ability to produce integrated complex parts
in a single step without the need for joining like welding. Selective laser
melting (SLM) is a powder-bed AM technique, in which a component is
produced by selectively melting consecutive layers of powder on top of
each other using a high-energy laser beam [1–3]. Upon irradiation, the
powder is melted and forms a tiny melt pool. This generates extremely
high temperatures up to 105 °C and rapid cooling up to 106-108 °C/s
within the melt pool [4,5]. The thermal history that materials experi-
ence during SLM processing is very different from that established by
conventional manufacturing techniques [6,7]. The rapid melting and
solidification in combination with cyclic heating and cooling upon the
deposition of subsequent layers result in a microstructure that differs
from traditionally-produced parts [8–10]. This has resulted in unusual
duced 316L stainless steel (hereafter 316L SS) [11].
It is well-known that an important microstructural characteristic of
a crystalline material that could be highly influenced by the thermal
history during the production process is the grain boundary (GB)
character. Such change in GB character could lead to changes in the IGC
behaviour of SLM-produced stainless steels. Research on IGC resistance
over the years has shown that the GB character has a crucial influence
on precipitation behaviour and IGC susceptibility [12–16]. Measure-
ments of GB character, with special emphasis on coincidence site lattice
(CSL) boundaries, have been the focus of GB engineering in improving
corrosion resistance. In spite of extensive studies on the microstructural
evolution and properties of SLM-produced 316L SS [17–22], the IGC
behaviour of SLM-produced stainless steels has yet to be studied in any
detail. A recent report has found that the SLM-produced 316L SS ex-
hibited a more rapid sensitization of GBs upon exposure to elevated
temperature compared to the wrought counterpart, however, the pre-
cipitation behaviour and its subsequent influence on the IGC resistance
are not well understood [23].
In the present study, an attempt was made to provide insight into
how the nonconventional thermal history associated with SLM pro-
cessing can influence the GB character, precipitation behaviour and IGC
susceptibility with the support of microscopy analysis and

⁎
Corresponding author at: Deakin University, School of Engineering, Faculty of Science and Technology, Geelong Waurn Ponds Campus, Waurn Ponds, Victoria,
3216, Australia.
E-mail address: mike.tan@deakin.edu.au (M.Y. Tan).

https://doi.org/10.1016/j.corsci.2019.108189
Received 24 May 2019; Received in revised form 14 August 2019; Accepted 28 August 2019
Available online 30 August 2019
0010-938X/ © 2019 Elsevier Ltd. All rights reserved.
M. Laleh, et al.
electrochemical measurements.
2. Experimental procedure
2.1. Materials and heat-treatment
Commercially available gas-atomized spherical 316L SS powder,
with a particle size range between 5 and 40 μm, was used to produce
specimens. Gas-atomisation was performed under argon gas atmo-
sphere. An SLM®-125HL machine was used to produce cubic specimens
with dimensions of 1.0 × 1.0 × 1.0 cm3. Prior to the SLM fabrication,
the build plate was pre-heated to a temperature of 200 °C and the build
chamber was purged with purified argon until the oxygen level was
reduced to below 100 ppm. The main processing parameters were laser
power of 150 W, scanning speed of 600 mm/s, hatch spacing of 80 μm
and layer thickness of 30 μm. The scanning pattern was bidirectional
with 67° angle between successive layers. The density of the SLM-pro-
duced specimens was 99.5 ± 0.1%, measured based on the
Archimedes method, using an electronic Densimeter (Model SD-200 L)
with 0.0001 g/cm3 resolution. The commercial (wrought) 316L SS was
received as 3 mm thick plate and then was solution annealed at 1100 °C
for 1 h followed by water quenching, prior to sensitisation studies [24].
Chemical composition of the SLM-produced specimen is presented in
Table 1, showing a comparable chemical composition with that of the
commercial counterpart. For the sensitisation experiments, the speci-
mens were heat-treated at 700 °C for 60 h and then immediately water
quenched.
2.2. Microstructural characterisation
For microscopy analysis, the specimens were mechanically polished
to a mirror finish with the last stage being a 0.3 μm oxide polishing
suspension (OPS). A scanning electron microscope (SEM ZEISS SUPRA
55 V FEG) equipped with an energy dispersive spectroscopy (EDS) de-
tector and operated at 20 kV was used for imaging and EDS analysis.
Transmission electron microscopy (TEM) was employed for a detailed
analysis of precipitates, using a JEOL JEM 2100 F microscope equipped
with an EDS detector and operated at 200 kV. EDS mapping was per-
formed in a scanning-transmission TEM (STEM) mode using a spot size
of 1 nm. For TEM analysis, thin slices with a thickness of approximately
500 μm were cut from the specimens and then mechanically ground to a
thickness of around 100 μm. Discs with a diameter of 3 mm were sub-
sequently punched from the slices and further ground using 4000
abrasive paper until their thickness was reduced to 60–70 μm. Final
thinning was carried out by twin-jet electro-polishing using a Struers
Tenupol 5 device. Electron backscatter diffraction (EBSD) acquisition
was performed using a ZEISS LEO 1530 FEG SEM, with a scan step size
of 0.3 μm at an accelerating voltage of 20 kV. Oxford Instruments Aztec
software was used for acquisition and indexing the EBSD patterns.
Further EBSD data post-processing was performed using HKL Channel 5
software. An area of 500 × 500 μm2 was used for EBSD analysis. A
ZEISS FEI QUANTA focused ion beam (FIB) SEM was used for milling of
cross-sections at grain boundaries.
2.3. Electrochemical tests
The sensitized specimens were evaluated for degree of sensitization
(DOS) using a double loop electrochemical potentiokinetic reactivation
Table 1
Chemical composition of the commercial and as-built SLM-produced 316L SS.
Element (wt%) C Cr Ni Mn Mo
Commercial 0.02 16.9 10.30 1.77 2.11
As-built SLM 0.02 16.6 11.60 1.11 2.70
2
Corrosion Science 161 (2019) 108189
(DL-EPR) test in 0.5 M H2SO4 + 0.01 M KSCN solution at room tem-
perature. For DL-EPR testing, firstly the potential was scanned in the
anodic direction from open circuit potential (OCP) to +0.35 V vs. the
reference electrode at a scanning rate of 100 mV/min and then im-
mediately reversed to the starting point at the same scanning rate. DOS
was reported as the ratio of maximum current density in the reactiva-
tion loop (Ir) to current density in the activation loop (Ia). The DL-EPR
experiments were repeated at least three times and the average values
of DOS are reported. After DL-EPR testing, the specimens were ex-
amined using optical microscopy (Olympus GX41) to analyse the in-
tergranular attack.
3. Results and discussion
In general, it is believed that the loss of intergranular corrosion
resistance at the GBs in stainless steels is due to the formation of GB
chromium carbides that cause localised Cr depletion in the region ad-
jacent to these precipitates [25–27]. The intergranular attack is be-
lieved to be accelerated by the increasing potential difference between
grain interiors (cathode) and GBs (anode). The DL-EPR test is a common
method for assessing such behaviour based on the assumption that only
the sensitised GBs become active, while grain interiors are unsensitised
[28,29]. Therefore, gaining further insight into the characteristics of
GBs and grain interiors as well as their correlation with the DL-EPR
behaviour is essential for a critical understanding of the IGC behaviour
of SLM-produced 316L SS.
As shown in Fig. 1, the EBSD analyses of the microstructures in the
commercial and SLM-produced 316L SS specimens reveals an obvious
difference in grain size and shape as well as the GB character. The
commercial 316L SS mostly comprised equiaxed grains (Fig. 1a).
However, grains in the SLM-produced specimen showed a fairly elon-
gated morphology on the build plane (parallel to the build direction), as
presented in Fig. 1b. The same specimen showed elongated grains se-
parated with melt pool boundaries when viewed from the transverse
plane (perpendicular to the build direction), as shown in Fig. 1c. The
mean grain size was measured to be 19.2 ± 0.7 μm, 8.4 ± 0.8 μm and
10.4 ± 0.9 μm for commercial, and SLM-produced specimens at
transverse and build planes, respectively, indicating a smaller grain size
for the SLM-produced specimens compared to their commercial coun-
terpart. The relative fraction and length of the GBs, measured from the
EBSD data, are summarised in Table 2 for all three microstructures.
Interestingly, these microstructures comprised a significant fraction of
∑3 boundaries and a relatively low fraction of ∑9 boundaries. A detailed
analysis of angle/axis pair associated with ∑3 boundaries (Brandon's
criterion [30]) revealed that almost 35%, 25% and 31% of commercial,
SLM-produced at transverse and build plane microstructures were of ∑3
character. As can be seen in the misorientation angle distribution plots
for the surfaces subjected to EBDS, the ∑3 peak at 60° is much sharper
for the commercial specimen. However, a relatively lower fraction of
the 60° boundaries is of a < 111 > misorientation axis in the com-
mercial microstructure compared to those in the SLM-produced speci-
mens. The same trend was observed for the misorientation axis peak
at < 110 > for the misorientation angle of 39°. This was not surprising
as a ∑9 boundary is dictated by the geometrical constraints of two in-
tersecting ∑3 boundaries [31].
It is important to note that an analysis of the misorientation angle
alone can be misleading in characterising the GB character [32]. Due to
the difference in the grain size, the length of different boundaries per
Si P S Nb Ti Cu Fe
0.50 0.04 0.01 0.03 < 0.01 0.39 Bal.
0.56 0.01 0.01 0.01 < 0.01 0.08 Bal.
M. Laleh, et al. Corrosion Science 161 (2019) 108189

Fig. 1. EBSD IPF maps (a,b,c) and band contrast maps (d,e,f) of the commercial specimen (a,d), SLM-produced specimen in the build plane (b,e), and in the
transverse plane (c,f). Z shows the build direction. The red and blue lines in (d–f) are ∑3 and ∑9 CSL boundaries, respectively. Misorientation angle/axis distribution
for the austenite/austenite boundaries for commercial specimen (g), SLM-produced specimen in the build plane (h), and in the transverse plane (i). The scale bars in
(a–f) are the same. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

Table 2 that of the commercial specimen, respectively. Hence, from the EBSD
Grain boundary characteristics for all three microstructures measured from the analysis, it is clear that the grain size and shape, as well as the GB
EBSD results presented in Fig. 1. character of the SLM-produced specimens are quite different from those
0.7° < θ < 2° 2° < θ < 15° 15° < θ ∑3 of their commercial counterpart, which is expected to influence the
precipitation behaviour during the sensitisation heat-treatment and
Commercial Fraction 1.0% 6.0% 92.5% 35.1% subsequent IGC resistance.
Length 394.80 μm 2.34 mm 3.58 cm 1.33 cm
Fig. 2 shows micrographs of the specimens after the sensitisation
SLM-produced Fraction 9.4% 4.7% 85.0% 24.8% heat-treatment, indicating the formation of precipitates along GBs. The
(transverse Length 8.23 mm 4.14 mm 7.45 cm 2.09 cm
dark spherical spots in Fig. 2b, c are inclusions, which are inherent in
plane)
austenitic stainless steels produced by SLM [11,18], and are not due to
SLM-produced Fraction 10.7% 4.0% 84.6% 31.3% the sensitisation heat-treatment. For the commercial 316L SS, coarse
(build plane) Length 8.39 mm 3.14 mm 6.63 cm 2.37 cm
precipitates were formed along GBs (Fig. 2a, d). STEM-EDS analysis
showed that these GB precipitates in commercial 316L SS are enriched
in Cr and C (Fig. 2d), indicating the formation of chromium carbides.
given area should also be considered in evaluating the GB character. It For the SLM-produced specimens, however, relatively fine precipitates
was revealed in Table 2 that the relative length of low-angle GBs are visible (Fig. 2b, c). Interestingly, the STEM-EDS analysis shown in
(2° < θ < 15°), which are of lower energy compared to their high-angle Fig. 2e reveals that these precipitates are indeed enriched in Mo and Si
counterparts, is approximately 75% and 35% higher in the micro- instead of Cr (Table 3), which can be considered as Laves phase. At first
structure of the SLM-produced specimens at the transverse and build glance, one may consider these precipitates in the SLM-produced 316L
plane surfaces, respectively, relative to the commercial specimen. The SS as sigma and chi phases, which are commonly found in duplex
lengths of the ∑3 boundaries measured at the transverse and build plane stainless steels when subjected to sensitisation heat-treatment [32–35].
surfaces of the SLM-produced specimen were 57% and 73% higher than In duplex stainless steels, these precipitates (sigma/chi) can quickly

3
M. Laleh, et al.
Fig. 2. SEM micrographs showing the precipitation along grain boundaries for commercial (a) and SLM-produced 316L SS at the transverse plane (b) and build plane
(c). The black spherical spots in (b,c) are the inclusions, which are inherent in stainless steels produced by SLM, and are not due to the sensitisation heat-treatment.
STEM images of the precipitates for the commercial (d) and SLM-produced (e) 316L SS specimens with their EDS elemental map analysis. The dark spot shown in the
dashed red line in (e) is the inclusion and is not due to the sensitisation heat-treatment. (For interpretation of the references to colour in this figure legend, the reader
is referred to the web version of this article.)
Table 3
STEM/EDS analysis of the precipitates in SLM-produced specimens after heat-
treatment at 700 °C for 60 h from Fig. 2.
Element (wt%) Fe Cr Mo Si
Laves phase 54.41 ± 0.32 16.15 ± 0.45 26.78 ± 0.65 2.67 ± 0.17
form when the Cr content is between 20 and 30%. Furthermore, the
sigma/chi precipitation tend to occur preferentially in the delta ferrite
islands [36]. But, based on the EBSD results, no delta ferrite was de-
tected for the SLM-produced specimens in our study, and the material is
a single-phase austenite. In addition, chemical compositional analysis
by STEM/EDS (Table 3) shows the enrichment of the Si in the pre-
cipitates in the SLM-produced specimens, which confirms these pre-
cipitates are Laves phase. This is in agreement with the literature,
where the presence of Si has been reported in the Laves phase [37–39].
More importantly, no chromium carbides were detected for the SLM-
produced specimens. So, the precipitation behaviour for commercial
and SLM-produced 316L SS is different under exposure to long-term
sensitisation heat-treatment.
For the additively manufactured 316L SS, the segregation of Mo in
the cell walls has already been shown in the literature [18]. One pos-
sible explanation for the formation of Laves precipitates in the SLM-
produced 316L SS might be the diffusion of Mo from the cell walls to
the GBs during the long-term sensitisation heat-treatment, which needs
further clarification in the future work. A similar explanation has been
made by Isik et al. [40], showing that segregation of Mo to grain
boundaries in steel can promote the formation of Laves phase during
high-temperature exposure.
To find the influence of precipitation on the IGC resistance, DL-EPR
tests were carried out, revealing a definite reactivation peak for the
commercial specimen, as shown in Fig. 3a. In contrast, DL-EPR analysis
of the SLM-produced specimens revealed no reactivation peaks. An
4
Corrosion Science 161 (2019) 108189
obviously higher DOS (25.7) was recorded for the commercial 316L SS
compared to those recorded for the SLM-produced specimens, i.e. 0.08
and 0.06 for transverse and build planes, respectively, as depicted in
Fig. 3b. The lack of reactivation peak for the SLM-produced specimens
indicates a minimal density of Cr-rich precipitates, in agreement with
the STEM-EDS compositional analysis (Fig. 2e). The high DOS in the
commercial 316L SS is consistent with the presence of Cr-rich pre-
cipitates shown in SEM and STEM images in Fig. 2. It seems that the IGC
resistance is mostly controlled by the Cr-rich (chromium carbides)
precipitates rather than Mo-rich (Laves) ones [41]. Optical microscopic
examination after DL-EPR measurements revealed a ‘ditch’ structure for
commercial 316L SS, where all the GBs were deeply corroded (Fig. 3c
and d). For the SLM-produced 316L SS specimens at both transverse
(Fig. 3e, f) and build (Fig. 3g, h) planes, the extent of attack at GB
regions is much less than that of their commercial counterpart.
To get a further insight into the corrosion attack along GBs, the
cross-section of the intergranular corrosion was examined using FIB-
SEM. Fig. 4(a–c) shows FIB images for the commercial specimen in-
dicating a substantial GB attack extending into the matrix (after the DL-
EPR test). By contrast, the GB attack for the SLM-produced specimens is
much less than that of their commercial counterpart. So, the extent of
the attack along the GBs correlates well with the DOS values estimated
from the DL-EPR curves; a higher DOS corresponds to a deeper attack
along GBs.
The results reported here show the substantially higher IGC re-
sistance of the SLM-produced specimens. When subjected to sensitisa-
tion between 500–850 °C, the formation of GB Cr-rich precipitates in
conjunction with the presence of Cr-depleted regions near GBs tends to
cause IGC in stainless steels [25–27]. Previous studies on the relation-
ship between GB characteristics and IGC resistance in stainless steels
have shown that only low-angle GBs and twin boundaries were immune
from being sensitised [15,42–46]. In the present study, the substantial
decrease in the degree of sensitisation of SLM-produced specimens can
M. Laleh, et al. Corrosion Science 161 (2019) 108189

Fig. 3. (a) DL-EPR curves for the commercial and SLM-produced 316L SS specimens recorded in 0.5 M H2SO4 + 0.01 M KSCN solution at room temperature; (b) DOS
values measured from the peak current densities of the forward and reverse scans in DL-EPR curves; optical images after DL-EPR tests for (c, d) commercial 316L SS
showing that all grain boundaries got severely attacked, and SLM-produced 316L SS at transverse (e, f) and build (g, h) surfaces, respectively, indicating a negligible
attack along grain boundaries.

Fig. 4. FIB cross-sections made on typical corroded grain boundaries to measure the depth of attack for (a–c) commercial and (d–g) SLM-produced 316L stainless
steel indicating an aggressive attack along the grain boundaries of the commercial specimen, and a slight attack for the SLM-produced 316L SS. The white rectangles
in (a, d, e) show the regions where the high magnification images in (b, c, f, g) were taken.

5
M. Laleh, et al.
be manifested in two ways viz. the smaller grain size and larger length
of CSL boundaries. It is believed that the degree of sensitisation has an
inverse relationship with the grain size [13,47]. The smaller the grain
size, the larger the total GB surface area, which in turn provides a larger
number of sites for precipitates to nucleate. However, the precipitates
need to attain a critical size to cause sensitisation. In the case of fine-
grained materials, such as the SLM-produced material in the present
study, the carbon availability for every single nucleus is restricted be-
cause of the higher number of nuclei and therefore chromium carbides
can’t precipitate, which is consistent with the observations in SEM and
STEM images in Fig. 2, where no trace of chromium carbides was de-
tected for SLM-produced specimens. Furthermore, the intergranular
corrosion was suppressed due to the uniform distribution of highly
coherent CSL boundaries, minimising the extent of intergranular cor-
rosion along the GBs [48], as indicated in the FIB sections in Fig. 4.
After subjected to the long-term sensitisation heat-treatment, the
SLM-produced specimens have substantially lower IGC susceptibility
compared to their conventionally-produced counterpart. Thermo-me-
chanical treatments have been usually applied to develop a maximum
proportion of low-angle GBs to improve the IGC resistance of austenitic
stainless steels, which is known as grain boundary engineering (GBE).
The results presented here show the potential of AM techniques in the
fabrication of IGC immune microstructures with finer grain size and
abundant CSL boundaries, without resorting to any post-processing.
Although GBE and its influence on the IGC resistance have been widely
studied for conventionally-produced stainless steels, tailoring GB
characteristics in situ via manipulation of the SLM processing conditions
opens a new avenue for the direct SLM manufacture of IGC resistant
316L SS components.
4. Summary
The IGC resistance of an additively manufactured 316L SS was
studied using a combination of microscopy analysis and electro-
chemical measurements. The relationship between the IGC and GB
character of the SLM-produced 316L SS was established for the first
time. No Cr-rich precipitates were detected for SLM-produced speci-
mens after a long-term sensitisation heat-treatment. Subsequently, DL-
EPR tests showed substantially lower DOS values for the SLM produced
316L SS compared to its commercial counterpart. Post-corrosion mi-
croscopy analysis revealed a continuous network of ditched GBs with
grooves extending deeply into the bulk in the case of commercial 316L
SS; while for the SLM-produced specimens, the attack along GBs was
less pronounced, indicating higher resistance of SLM-produced 316L SS
to IGC. This behaviour was found to be related to the GB character,
where the SLM-produced specimens exhibited a high frequency of twin
boundaries and low-angle GBs along with fine grains.
Data availability statement
The raw/processed data required to reproduce these findings cannot
be shared at this time as the data also forms part of an ongoing study.
Acknowledgement
Financial support from Deakin University Postgraduate Research
Scholarship (DUPRS) is greatly appreciated. Deakin University’s
Advanced Characterisation Facility is acknowledged for use of the mi-
croscopy instruments and assistance from Dr Adam Taylor and Dr Mark
Nave.
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