Acta Materialia 242 (2023) 118481

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Acta Materialia
journal homepage: www.elsevier.com/locate/actamat

Full length article

Effects of initial 3D printed microstructures on subsequent

microstructural evolution in 316L stainless steel
Chunlei Zhang∗, Dorte Juul Jensen, Tianbo Yu∗
Department of Civil and Mechanical Engineering, Technical University of Denmark, Kgs. Lyngby DK-2800, Denmark

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

Article history: Plastic deformation of 3D printed components may occur when they are in use. Here we analyze the
Received 23 June 2022 effects of the initial 3D printed microstructure of 316 L stainless steel on the subsequent deformation be-
Revised 2 September 2022
havior, where we apply 10% and 30% thickness reductions by cold rolling. The microstructures are charac-
Accepted 24 October 2022
terized by electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM). Compared
Available online 25 October 2022
to conventionally manufactured (solution treated) samples, deformation twinning is observed to occur at
Keywords: lower strains in 3D printed samples, and twins are observed to be thinner and intersecting inside some
3D printed 316L grains. These observations are linked to the pre-existing dislocation structure in the 3D printed samples,
Cold rolling where dislocations of various Burgers vectors facilitate deformation twinning. Furthermore, cells with an
Microstructure average size of 125 nm are observed to form inside the initial cellular structure. The strength calcu-
Deformation twinning lated based on microstructural parameters generally agrees with experimental results, showing a large
Mechanical properties
strengthening contribution from twin–matrix lamellae. The present study provides fundamental ideas for
microstructural engineering of 3D printed metals for even better mechanical properties.
© 2022 The Author(s). Published by Elsevier Ltd on behalf of Acta Materialia Inc.
This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/)

1. Introduction
Metal 3D printing, a popular additive manufacturing (AM) pro-
cess, has drawn enormous attention during the last few decades
because it enables near net-shape manufacturing of components
with complex shapes [1–3]. Laser powder bed fusion (L-PBF) is
in particular popular. This technology has been used to manufac-
ture components of many alloys, e.g., Ti-6Al-4 V, TiAl-based al-
loys, Inconel 718, AlSi10 Mg, and stainless steels [2,4–6]. Austenitic
stainless steel 316 L is one of the most frequently used stainless
steels, due to its good corrosion resistance and formability. Many
316 L components have complex geometries, for example pipeline
systems used in the nuclear industry [7], various tailor-made im-
plants [8,9], and structural components used in the automotive and
aerospace industries [10], making conventional manufacturing pro-
cesses difficult and costly. Additionally, a promising result is that
316 L samples produced by L-PBF may have even better mechanical
properties (higher strength and comparable ductility) than those of
as the cast and even wrought counterparts [11,12]. Thus, there is
huge potential in producing 316 L components via AM techniques
and a need for understanding the relationship between AM param-
eters, microstructure, and mechanical properties.
∗
Corresponding authors.
E-mail addresses: chzhang@mek.dtu.dk (C. Zhang), tiyu@dtu.dk (T. Yu).
Extensive recent research has shown that the printing parame-
ters, for example the scan strategy, laser power, and scan speed,
significantly affect the microstructure, porosity distribution, and
mechanical properties of printed samples, e.g., [13–15]. With care-
ful optimization of the printing parameters, almost fully dense
printed samples with reproducible microstructures can be obtained
[16,17]. When a melt pool is cooling down, the <001> crystallo-
graphic direction is favored for growth along the maximum tem-
perature gradient (in metals of cubic crystal system), which is nor-
mally perpendicular to the melt pool surface [18]. Therefore, the
texture of the printed components can be controlled by manip-
ulating the printing parameters and thus the melt pool geome-
try during printing. For example, Sun et al. [18] reported that by
optimizing the laser power and scan strategy, the texture of the
printed materials is highly dependent on the depth of the melt
pool; <100> texture tends to form in shallow melt pools while
<110> texture tends to form in deep melt pools. In addition, ma-
terials with <110> and <100> texture have been manufactured by
utilizing the unidirectional scanning and 90° rotation between ad-
jacent layers, respectively [19,20]. The texture induced by printing
can affect the deformation behavior and thus also the strength and
ductility of the printed components; deformation twinning tends
to occur in domains with <011> texture under tensile loading [18].
For industrial applications, the scanning strategy of 67° laser ro-
tation is usually applied to avoid a strong texture and to make

https://doi.org/10.1016/j.actamat.2022.118481
1359-6454/© 2022 The Author(s). Published by Elsevier Ltd on behalf of Acta Materialia Inc. This is an open access article under the CC BY license
(http://creativecommons.org/licenses/by/4.0/)
C. Zhang, D. Juul Jensen and T. Yu
the directions in the scanning plane (normal to building direction)
equivalent.
This improvement in mechanical properties of 3D printed
samples/components is generally attributed to the fine-scale mi-
crostructures resulting from the printing process. Wang et al.
[17] reported a complex heterogeneous cellular microstructure in
printed 316 L samples and suggested this as an explanation for the
improved properties. A recent study [21] suggests that it is the lo-
cal thermal expansion/shrinkage in a constrained medium which
gives rise to the formation of the cellular structure, rather than
other factors, e.g., dendritic micro-segregation and the resultant
constitutional stress, or misorientations between dendrites. Some-
times also a cellular structure is observed. It is worth noting that
the cellular/columnar structure is actually cylindrical in 3D and the
difference between seeing a cellular or a columnar structure is due
to different viewing directions, i.e., it is a stereological effect [22].
Irrespective of how the pre-existing cellular/columnar structure is
formed, it is expected to affect the dislocation behavior, and there-
fore plays a vital role, in any subsequent deformation process.
There has been extensive research, investigating the deforma-
tion behavior of 3D printed 316 L, e.g., [17,23,24], mainly focus-
ing on the analysis of the tensile behavior. It is suggested that
the finely-spaced cellular/columnar boundaries together with ele-
mental segregation facilitate dislocation storage and deformation
twinning, contributing to the high strength and good ductility of
3D printed 316 L [17,25]. Moneghan et al. [26] suggested that
the cellular/columnar structure can delocalize the strain and thus
increase the defect tolerance. In-situ transmission electron mi-
croscopy (TEM) observations revealed that the cellular/columnar
boundaries are weak obstacles to both dislocation motion and de-
formation twinning [12]. The high temperature evolution of the
cellular/columnar structure has also been analyzed [27]; the cel-
lular/columnar structure appears to be stable up to 600 °C, below
which the yield strength also appears to be unchanged, ensuring
the properties of the printed components are maintained in a wide
temperature range.
These are all detailed investigations. However, to the best of au-
thors’ knowledge, there is a lack of quantitative TEM characteriza-
tion of how the 3D printed microstructures (particularly the cel-
lular/columnar structure) evolve during subsequent deformation.
Such high fine-scale characterization, we consider essential for
understanding the evolution of microstructures and properties of
components when they are mechanically loaded while in-service,
and for providing guidance for the practical application of printed
components. The present study aims at providing such a detailed
microstructural characterization. Regarding the deformation mode,
we have here chosen cold rolling. It is of course clear that a printed
component is not expected to be rolled for, or in, a practical ap-
plication. In spite of this we have chosen to study rolling of 3D
printed 316 L, because the microstructural evolution of conven-
tionally manufactured (solution treated) 316 L during cold rolling
is well known [28]. By comparing the two sets of microstructures
as a function of strain, it is thereby possible to directly quantify
the effects of the printing microstructures on the subsequent de-
formation behavior—for example the balance between deformation
twinning and dislocation slip—and its effects on the evolution of
mechanical properties.
2. Experimental
Stainless steel 316 L samples, with sizes of 3 × 4 × 14 mm in
the scanning directions X, Y and the building direction (BD), were
produced by L-PBF. The laser power and scanning speed were set
to 370 W and 1.35 m/s, respectively. A 67° rotation of the scanning
direction between neighboring layers was applied, making the X
and Y scanning directions equivalent. To improve the surface fin-
2
Acta Materialia 242 (2023) 118481
Fig. 1. Sketch of the rolling geometry of the as printed sample (P-0). The rolling
direction (RD) is parallel to the building direction (BD); the normal direction (ND)
is parallel to the X direction; the transverse direction (TD) is parallel to the Y direc-
tion. The small micrographs in the longitudinal section (LS) and the cross section
(CS) indicate the sections used for microstructural characterization.
ish of the component, a final contour scanning, with input power
of 120 W and scanning speed of 0.22 m/s, was applied. The as
printed microstructure was characterized by electron backscatter
diffraction (EBSD) and TEM. The results hereof are summarized in
Supplementary materials S1.
As sketched in Fig. 1, the 3D printed samples were unidirection-
ally rolled along BD at room temperature to thickness reductions
of 10% and 30% (von Mises equivalent strains ε vm of 0.12 and 0.41,
respectively). During cold rolling, the samples were lubricated by
mineral oil and turned upside down between each pass. The ratio
of the contact length to the mean height l/h was kept at about one
to ensure through-thickness strain homogeneity. For convenience,
the as printed sample, and the printed samples after 10% and 30%
thickness reductions are denoted as P-0, P-10%, and P-30%, respec-
tively.
A Zeiss Supra 35 field emission gun scanning electron micro-
scope (FEG-SEM), equipped with an HKL EBSD system, was used
to characterize the microstructure. EBSD samples were prepared by
grinding using SiC papers followed by mechanical polishing. A col-
loidal silica suspension (0.04 μm) was used for the final polishing
step. TEM investigations were performed using a JEOL JEM-2100
microscope at an acceleration voltage of 200 kV. Foils for the TEM
investigations were prepared by a modified window technique in
a perchloric acid based electrolyte [29]. EBSD and TEM characteri-
zations were carried out at the thickness center in both the cross
section and the longitudinal section (see Fig. 1). EBSD maps were
obtained using a step size of 500 nm. Simple noise reduction, e.g.,
removing wild spikes and filling them with neighbor orientations,
was applied using Channel 5 software. MTEX was used for analyz-
ing the EBSD data [30,31], e.g., the Schmid factor analysis. EBSD
orientation maps are in the present study colored according to the
normal direction to the observation surface in the inverse pole fig-
ure. We have chosen 15° as the cutoff misorientation angle because
this is the value we used for the analysis of conventionally manu-
factured samples, and we define boundaries in EBSD maps accord-
ing to their misorientation angles into low angle boundaries (LABs,
2–15°) and high angle boundaries (HABs, >15°). Twin boundaries
are defined as boundaries which deviate less than 2° from the
misorientation angle/axis of 60°/<111>. The Vickers microhardness
was measured using a Struers DuraScan hardness tester with a
load of 300 g. For all samples, the hardness was measured in the
longitudinal section, and each value was averaged over at least 12
measurements. Larger samples for tensile test with the dimensions
130 × 12 × 3 mm were printed using the same printing parame-
ters. Some of these larger samples were cold rolled to 30% thick-
ness reduction before they were cut into dog-bone shaped speci-
mens. The tensile tests were done using a universal tensile testing
machine at a strain rate of 4 × 10−4 .
C. Zhang, D. Juul Jensen and T. Yu
Fig. 2. Inverse pole figure coloring maps of P-10%. (a) Longitudinal section (TD col-
ored); (b) cross section (RD colored). The thick black lines mark twin boundaries;
gray lines and thin black lines mark LABs and other HABs, respectively. The black
arrows in (b) mark the grains with double sets of deformation twins.
3. Results
3.1. Microstructure after 10% thickness reduction (P-10%)
After 10% thickness reduction, deformation twins are observed
in EBSD orientation maps as shown in Fig. 2. There is no obvious
change in the shape of grains (here domains delineated by HABs
are denoted as grains for simplicity although they appear different
from grains in conventionally manufactured materials) after defor-
mation compared to that of P-0 (see Supplementary materials S1).
In total, 14% of the grains (area fraction) are observed to have de-
formation twins at this strain. Most of the grains hosting twins ex-
hibit a single set of deformation twins, only two grains are ob-
served exhibiting double sets of deformation twins (marked by the
black arrows in Fig. 2(b)). The fraction of twin boundaries is 5%,
while LABs amount to 67%, of the total boundary length (see Sup-
plementary materials S2).
It is a common observation that deformation twins penetrate
and shear the columnar dislocation boundaries (CoDBs) after 10%
cold rolling, as shown in Fig. 3(a). In the region delineated by
CoDBs, the dislocation density increases due to plastic deforma-
tion. In a few grains where two sets of deformation twins are
observed, the grains are subdivided into many parallelogrammatic
regions (see Fig. 3(b)). A high density of dislocations is also ob-
served in these parallelogrammatic regions, further subdividing the
microstructure by forming new dislocation boundaries. For some
CoDBs, e.g., the CoDB marked by the white dashed line in Fig. 3(c),
some deformation twins are stopped by the boundaries (see white
arrows in Fig. 3(c)) although others penetrate the boundaries (see
red arrows in Fig. 3(c)), indicating the moderate effect of CoDBs
on deformation twinning. Twins are also seen in the cellular dis-
location boundaries (CeDBs) structure. A magnified image, exhibit-
ing double sets of deformation twins formed on two {111} planes,
is shown in Fig. 3(d). The vertical set develops first and is thus
sheared by the subsequent deformation twinning set. The latter is
a twin bundle containing multiple thin deformation twins. A high
dislocation density inside the twin bundle is observed. Typical dis-
location structures observed in areas without deformation twins
are shown in Fig. 3(e, f). Some dislocations align on one of the
{111} planes as marked by the white dashed lines in Fig. 3(f). How-
ever, a common observation is that rolling induced dislocations en-
tangle and organize to form new dislocation boundaries between
the original CeDBs/CoDBs.
3.2. Microstructure after 30% thickness reduction (P-30%)
After 30% thickness reduction, an elongated microstructural
morphology is observed (compressed along ND) as shown in Fig. 4.
The aspect ratio, i.e., the spacing of HABs along RD or TD to that
along ND, increases to 3 in the longitudinal section and to 1.5 in
the cross section (Fig. 4(a, b)). More grains (31% in area fraction)
3
Acta Materialia 242 (2023) 118481
are observed to deform by twinning, compared to P-10% (14%). The
fraction of twin boundaries increases to 15% of the total bound-
ary length (see Supplementary materials S2). Twin boundaries are
at a tilt of ±45° to RD in the longitudinal section (Fig. 4(a)) and
parallel to TD in the cross section (Fig. 4(b)). These twin planes,
approximately ±45° rotated about TD from the rolling plane, are
close to the planes of the largest resolved shear stress. Although
single sets of deformation twins are still the most common obser-
vation, double sets are also frequently observed, as marked by the
white arrows in Fig. 4(a).
An example of a TEM observation of a grain with double sets of
deformation twins is shown in Fig. 5(a1). The first set of twins is
thinner and more narrowly spaced compared to the second set of
another twin variant, indicating that the first set of twins are fa-
vorable under the current stress state. The high magnification im-
age in Fig. 5(a2) shows very thin deformation twins with thick-
nesses down to a few nanometers. Microbands are commonly ob-
served after 30% thickness reduction, and an example is shown in
Fig. 5(b1). Microbands form by different combinations of slip sys-
tems or different partitioning of slip on the same slip systems in
neighboring parts of the microstructure, and thus the orientations
on the two sides are different. In the present sample, the misori-
entation angles across the microbands are low, typically less than
5°, and microbands are observed to strongly interact with deforma-
tion twins. As a result, twins are commonly observed to be sheared
by microbands especially in the longitudinal section as shown in
Fig. 5(b2).
Fig. 5(c1) shows an example of a deformation twin penetrat-
ing through pre-existing CeDBs. The misorientation of the twin
boundary is found to differ from the perfect 60°/<111> due to
subsequent deformation (the misorientation angle is observed to
be 48°). Although it appears to be rather ‘clean’ inside the twin
in the current view, dislocation boundaries are observed when the
sample is tilted to a proper position. A few stacking faults, aligned
parallel to the deformation twin, are also observed (see Fig. 5(c1)).
Another example is shown in Fig. 5(c2), exhibiting double sets of
twins intersecting with each other inside the cellular structure,
e.g., at the CeDBs marked by the white dashed line. Fig. 5(c3)
shows an example of extensively developed deformation twins in-
side the cellular structure, which is marked by the white dashed
lines. Most deformation twins are observed to penetrate the CeDBs
while some are stopped by the CeDBs as marked by the arrows in
Fig. 5(c3).
Fig. 6 shows an example of the typical dislocation structure
in areas without deformation twins. There is a high density of
dislocations between the pre-existing CoDBs/CeDBs. As shown in
Fig. 6(a), these dislocations start to organize into new cells of
smaller size (rolling-induced cells) than that of the pre-existing
dislocation structure. Fig. 6(b) shows interaction between CeDBs
and dislocations activated during cold rolling, increasing the width
of CeDBs as well as the overall dislocation density.
3.3. Mechanical properties
The hardness measured on the longitudinal section is shown
in Fig. 7(a), revealing a significant increase by cold rolling. Also
shown is the hardness variation of conventionally manufactured
316 L samples during cold rolling (denoted as C-0, C-10%, C-30%
and C-50%) from a previous study [28] for comparison. The hard-
ness of P-0 is considerably higher than that of C-0, indicating high
strength of 3D printed samples. The hardness of P-0 is comparable
to that of C-10%, suggesting that the strengthening effect of the 3D
printing process is similar to that of 10% cold rolling although the
two microstructures are significantly different. The hardness of P-
30% is more than 350 Hv, which is comparable to that of C-50%.
The yield strength of the printed sample is increased by 79% after
C. Zhang, D. Juul Jensen and T. Yu
Fig. 3. TEM images showing the deformation microstructure of P-10%. (a) Longitudinal section view, showing deformation twins (DTs) penetrating CoDBs; (b) cross section
view, showing the interactions between double sets of deformation twins, dislocation boundaries, and loose dislocations; (c) cross section view, showing the interaction
between deformation twins and CoDBs (the white arrows mark twins that are stopped by the CoDB while the red arrows mark twins penetrating the CoDB); (d) cross section
view, showing double sets of deformation twins (inset is the diffraction pattern taken from an intersection area of the two sets of twins); (e, f) typical microstructures in
grains without deformation twins.
Fig. 4. Inverse pole figure coloring maps of P-30%. (a) Longitudinal section (TD col-
ored); (b) cross section (RD colored). Thick black lines mark twin boundaries; gray
lines and thin black lines mark LABs and other HABs, respectively. The white ar-
rows mark examples of double sets of twins. The grains are elongated along RD.
More deformation twins are detected compared to samples deformed to a lower
strain.
30% cold rolling (from 500 to 895 MPa), although the ductility is
severely reduced simultaneously (see the tensile curves in Fig. 7b).
To estimate and compare the work hardening rate of the printed
and conventionally manufactured samples, the stress–strain curves
are fitted by the standard Voce model [32] based on the hard-
ness data (see Supplementary materials S3 for details about the
fitting), showing a vertical shift (Fig. 7c). The work hardening rate
of the printed samples is higher than that of conventionally man-
ufactured ones at the same stress level (see Fig. 7d).
4. Discussion
4.1. Deformation of 3D printed 316L samples
After printing of 316 L samples, the microstructure consists of
grains of rather irregular shapes (micrometer scale) each subdi-
4
Acta Materialia 242 (2023) 118481
vided by CeDBs/CoDBs (sub-micron scale). This microstructure (see
Supplementary materials S1) is significantly different from those
in the initial state and cold rolled state of conventionally manufac-
tured 316 L and is expected to affect the subsequent deformation
behavior. It is therefore of relevance to analyze the deformation
behavior by comparing the microstructural evolution during defor-
mation in printed samples to that in conventionally manufactured
samples. In the present work, the focus is on deformation by cold
rolling. The microstructural evolution during cold rolling of con-
ventionally manufactured samples has been systematically char-
acterized previously [28], and can be summarized in brief as: At
small strain (10–30% cold rolling), a Taylor lattice structure forms
due to planar slip of dislocations. Microbands start to form after
30% cold rolling, accommodating a high density of dislocations.
Only few deformation twins form at low strain (10% cold rolling),
while the volume fraction of twins increases with increasing strain
up to 50%, forming twin–matrix lamellae. As deformation twin-
ning occurs later than microband formation, it is observed that
microbands are sheared by the subsequent twinning after 30% cold
rolling. It was furthermore found that deformation twinning occurs
preferentially in grains with Copper orientation rather than Brass
orientation and largely on planes with the highest Schmid factor
for twinning. These results from conventionally manufactured sam-
ples serve as a basis for the analysis of the results obtained in the
present study.
4.1.1. Dislocation activity
In contrast to the conventionally manufactured samples, Taylor
lattice structures are not observed to form during cold rolling in
the 3D printed samples. In 316 L, planar slip of dislocations pre-
vails during cold rolling [28,33] due to its low stacking fault en-
ergy. Therefore, at low strains, dislocations are activated and glide
on one or two favorable {111} slip planes, forming the Taylor lattice
C. Zhang, D. Juul Jensen and T. Yu Acta Materialia 242 (2023) 118481

Fig. 5. Bright field TEM images showing the morphology of deformation twins (DTs) in P-30%. Panel (a) shows double sets of deformation twins. (a1) Overview of double sets
of deformation twins inside a grain; (a2) a magnified image showing twin–twin interaction. Panel (b) shows the interaction between dislocations and deformation twins. (b1)
In a columnar structure; (b2) in a cellular structure. Panel (c) shows details of deformation twins in the CeDB structure. (c1) Cross section view, showing one deformation
twin developing in a cellular structure and some stacking faults (SF) parallel to the deformation twin; (c2) cross section view, showing double sets of twins intersect with
each other at the CeDBs, as marked by the white dashed line; (c3) longitudinal section view, showing finely spaced deformation twins in one cellular structure. The white
dashed lines mark the CeDBs.

Fig. 7. Mechanical properties. (a) Microhardness measured in the longitudinal sec-

Fig. 6. Microstructure of areas without deformation twins in P-30%. (a) Formation
of rolling-induced dislocation cells in the columnar structure. (b) Loose dislocations
seen inside the cellular structure.
tion (RD/ND plane) of 3D printed and conventionally manufactured samples as a
function of deformation strain. The error bars represent standard deviations. (b)
Engineering stress vs strain curves for P-0 and P-30%. (c) The stress–strain curves
fitted by the standard Voce model based on hardness data (see Supplementary ma-
terials S3 for details about the fitting). Note the error bars here represent standard
errors. (d) Work hardening rate vs stress based on the fitted stress–strain curves.

actions between dislocations. In areas without deformation twins,

structure in conventionally manufactured 316 L. However, in the small cells form within the pre-existing cellular/columnar structure
3D printed 316 L, the pre-existing dislocation structure with vari- to accommodate the increasing dislocation density, e.g., Fig. 6. Af-
ous Burgers vectors acts as both a source and an obstacle [17] to ter 30% cold rolling, the average size of these cells is about 125 nm
the dislocation motion (see Figs. 3 and 6), leading to more inter- (see Fig. 8), i.e., on average one quarter of the original CeDB/CoDB

5
C. Zhang, D. Juul Jensen and T. Yu
Fig. 8. The size distribution of dislocation cells in P-30%. The average cell size is
about 125 nm, a quarter of the original CeDB spacing.
spacing. It is worth noting that such new cells were not observed
in P-10% or in cold rolled conventionally manufactured 316 L [28].
4.1.2. Deformation twinning behavior
Compared to the conventionally manufactured samples, twin-
ning starts from a lower strain and occurs more extensively in 3D
printed samples during deformation. In P-10%, deformation twin-
ning can be detected by EBSD using a step size of 500 nm whereas
it is not detectable in C-10% using the same step size. This trend
continues and after 30% cold rolling, deformation twinning occurs
more extensively in P-30% than in C-30% with the fraction of twin
boundaries 72% vs 60% (P-30% vs C-30%) of the total high angle
boundary length. It has been reported that deformation twinning
is affected by deformation temperature, strain rate, stacking fault
energy, and grain size [34]. The first three factors cannot explain
the present results as they are similar in the two cases. Concern-
ing the grain size effect, it is generally accepted that larger grains
favor deformation twinning [34], although this effect is small for
face-centered-cubic (FCC) metals [35]. The average grain size of the
conventionally manufactured 316 L investigated is about 26 μm
[28] while it is 25 μm (33 μm/17 μm along BD/X) in the present
printed sample, suggesting that the grain size cannot explain the
difference in deformation twinning in the present case.
It follows that the pre-existing dislocation structure has a ma-
jor effect on deformation twinning. The dislocations in the pre-
existing dislocation boundaries are mostly dissociated partial dislo-
cations with the Burgers vector 1/6<112> [12]. Experimental evi-
dence is shown in Figure S2 in Supplementary materials, where the
partial dislocations glide from one side of a cell to the other side,
forming a stacking fault in between during printing. Since partial
dislocations and stacking faults can serve as nucleation sites for
twinning [34], it is thus reasonable to expect earlier and more ex-
tensive deformation twinning upon external loading as observed in
the present study. However, the pre-existing dislocation structure
could also act as a weak obstacle to the growth of the deformation
twins [12,17]. As mentioned above, some deformation twins are
observed to penetrate the dislocation structures while others are
stopped (see Fig. 3). This is attributed to the interaction between
twinning partial dislocations and the pre-existing dislocation struc-
ture. When a twinning partial encounters a CeDB/CoDB, it may
be repelled by the dislocation boundary and only breaks through
upon further loading (larger stress). This has been observed by in-
situ TEM [12]. Another possibility is that the twinning partial may
be trapped by the dislocation boundary through the formation of
6
Acta Materialia 242 (2023) 118481
Fig. 9. The twin thickness in 3D printed samples (P-10% and P-30%) and in conven-
tionally manufactured samples (C-10% and C-30%). Note that the scale of X-axis for
C-30% is different from others. The average twin thickness and standard deviations
are given. The average twin thickness for the printed samples is smaller than that
for the conventionally manufactured samples.
Lomer–Cottrell locks:
a   a a
112̄ + [112] = [110]
6 6 3
In the printed samples, there are a large amount of partial dis-
locations with various Burgers vectors of the type a/6<112>, which
would react with twinning partials to form such Lomer–Cottrell
locks with the Burgers vector a/3<110> to reduce the disloca-
tion energy. These dislocations do not easily glide in FCC metals
at room temperature due to a large Peierls–Nabarro stress [36].
Therefore, twinning cannot continue in this case. Upon increas-
ing strain, the Lomer–Cottrell locks can cause stress concentration,
thereby initiating another partial dislocation. If this partial disloca-
tion inherits the initial Burgers vector, the twinning may continue.
If a new partial is initiated, then a new twinning variant can form
provided the shear stress is large enough for the growth of the
new twins, contributing to the frequently observed double sets of
twinning in 3D printed 316 L samples.
The present results suggest that the pre-existing dislocation
structure can also affect the morphology of deformation twins.
Thinner deformation twins (average thickness) are observed in 3D
printed 316 L than those in conventionally manufactured samples
after deformation (see Fig. 9). Furthermore, the median of twin
thickness for printed samples is also smaller than that of conven-
tionally manufactured samples (see Supplementary materials S4
for details). Through two-sample t-Test, it is concluded that the dif-
ference between the twin thicknesses of the 3D printed and con-
ventionally manufactured samples is significant within 95% con-
fidence. One may argue that the difference in the thickness and
density of deformation twins may be caused by the difference in
stress level between printed samples and conventionally manufac-
tured samples. However, the t-Test results (Fig. S4(c, d) in Sup-
plementary materials) for twin thicknesses of both printed sam-
ples (P-10% vs P-30%) and conventionally manufactured samples
(C-10% vs C-30%) show that there is no significant difference in
average twin thickness at strains from 10 to 30%, suggesting that
the stress level, at least in this strain range, has no obvious effect
on the twin thickness. It is therefore suggested that it is the cellu-
lar structure, containing a high variety of partial dislocations, that
provides nucleation sites for twinning (ether by providing stack-
ing faults or by providing twinning partial dislocations) and in-
creases the twinning nucleation probability, resulting in more ef-
ficient stress release, as well as thinner and denser deformation
twins. Liu et al. [12] presented evidence of deformation twins with
C. Zhang, D. Juul Jensen and T. Yu
Fig. 10. Difference between grains with twins and without twins in P-30%. (a, c)
Orientation map and {111} pole figure of grains with twins in P-30% (Fig. 4(a)). (b,
d) For grains without twins. (e) The highest Schmid factor for twinning (mt ). (f)
Ratio of the highest Schmid factor for twinning (mt ) to the highest Schmid factor
for slip (ms ), i.e., (mt /ms ). The grains with twins show an orientation away from
Copper orientation; the grains without deformation twins show an orientation near
Brass orientation. There is no obvious difference in the highest Schmid factor for
twinning between grains with twins and grains without twins, whereas the ratio of
Schmid factors (mt /ms ) is higher for grains with twins.
thicknesses ranging from 2 to 6 nm observed during in-situ ten-
sile tests. This is thinner than those observed in the present study,
probably due to the difference in deformation condition.
4.2. Orientation dependence of deformation twinning
In conventionally manufactured and cold rolled samples, defor-
mation twinning is found to be orientation dependent [28]. In the
3D printed samples, we have observed that grains with Brass ori-
entation are not favorable for twinning (see Fig. 10), similar to the
results for conventionally manufactured samples. However, many
grains with twins in 3D printed samples have an orientation away
from the Copper orientation (see Fig. 10(c)), which is the favorable
orientation for twinning in conventionally manufactured samples.
To understand this difference, a Schmid factor analysis is done. The
Schmid factor for rolling is defined [37] as:
(cosϕRD cosγRD − cosϕND cosγND )
m=
2 perimental observations.
where ϕ RD and ϕ ND are the angles between the slip/twinning
plane normal and RD and ND, respectively; γ RD and γ ND are the
angles between the slip/twinning direction and RD and ND, respec-
tively. The results show no apparent difference in Schmid factors
for twinning (mt ) between grains with twins and without twins
in the printed sample (see Fig. 10(e)). However, higher average ra-
tio of Schmid factors, i.e., mt /ms (ms denotes the Schmid factor for
slip), is observed for the grains with twins (see Fig. 10(f)). Similar
results were obtained from conventionally manufactured samples.
7
Acta Materialia 242 (2023) 118481
It is worth noting that there is large overlap between the distri-
bution of mt /ms for grains with twins and that for grains without
twins as shown in Fig. 10(f). This is due to the high symmetry of
FCC metals, resulting in many equivalent slip/twinning systems.
Another difference found is that all the deformation twinning
detected by EBSD occurs on the planes having the highest mt in
C-30% whereas only 13/19 (13 grains out of 19) exhibits the same
pattern in P-10% and this probability decreases to 31/100 in P-30%.
These phenomena suggest that in 3D printed samples, twinning se-
lection is a more complex process than that in conventionally man-
ufactured samples due to the effects of the pre-existing dislocation
structure and irregularly shaped grains.
For the case of double sets of deformation twins, one set of
twins develops on the plane with the highest mt while the other
set develops on a plane with very low mt (near zero). As a shear
stress is needed for the motion of partial dislocations on the twin-
ning plane for twinning propagation if the classic twinning the-
ory is correct [34], large internal stresses are expected in the 3D
printed samples with irregularly shaped grains and pre-existing
dislocation structures. Both the irregularly shaped grains and pre-
existing dislocation structures can cause a complex local stress
state and therefore provide the resolved shear stress required for
the development of deformation twins on planes other than the
one with the highest mt during the subsequent cold rolling. How-
ever, further understanding of this phenomenon requires more in-
formation on relations between the 3D microstructure and the lo-
cal stress, which may be obtained by advanced experimental stud-
ies using the 3DXRD technique [38].
4.3. Microstructure–property relationship
As has been analyzed above, the large variety of Burgers vectors
of pre-existing dislocations leads to a more uniform deformation
and thinner twins in 3D printed samples than in conventionally
manufactured ones. Deformation twinning has been considered as
a mechanism to achieve a good strength–ductility combination for
metals, known as twinning induced plasticity (TWIP) [39,39–43].
This is because deformation twinning decreases the spacing of high
angle boundaries (HABs), resulting in a high work hardening rate
due to the dynamic Hall–Petch effect and thus good ductility [44–
46]. Due to the strong twin–dislocation interaction (as has been
extensively studied, e.g., [47–50]), twin boundaries of 60°/<111>
will gradually evolve into ordinary high angle boundaries with in-
creasing deformation strain [51], as shown in Fig. 5(b1, b2). In ad-
dition, rolling-induced cells, a novel phenomenon observed in the
present work, are rarely reported in the literature for 3D printed
316 L after deformation, and their strengthening effect has not
been considered in the analysis of the mechanical properties. The
twin–twin, twin–dislocation and dislocation-dislocation boundary
interaction may affect the ductility and the work hardening rate of
the printed samples during deformation [45,52,53]. To understand
the strengthening effect of the pre-existing cellular/columnar dis-
location structure and the subsequent deformation microstructure,
the microstructural parameters of both printed and conventionally
manufactured samples (for comparison) are quantified, and their
strengthening contributions are analyzed and compared with ex-
On the assumption of additivity of the strength contribution
from dislocation structures (dislocations in low angle dislocation
boundaries plus loose dislocations, i.e., those not organized into
low angle boundaries) and high angle boundaries [45], the flow
stress σ at strain ε may be expressed by the following equation:
 √
σ (ε ) = σ0 + Mα G 1.5(SV θ )b + ρ0 b2 + K1 / D (1)
where σ0 is the frictional stress, including contributions from so-
lutes and particles, independent of grain size; M is the Taylor fac-
C. Zhang, D. Juul Jensen and T. Yu Acta Materialia 242 (2023) 118481

Table 1
Constants used for the calculation of strength.

b α G K1 σ0 KT −M (= K1 )

0.254 nm 0.2 77 GPa 299 MPa·μm1/2 [55] 173 MPa [55] 9455 MPa·nm1/2

Table 2
Microstructural parameters and yield strength (both calculated and experimentally measured).

M SV θ D ρ0 ρ0T −M f T −M λ σcal σexp

(μm−1 ) (o ) (μm) (1014 m−2 ) (1014 m−2 ) (%) (nm) (MPa ) (MPa )
P-0 3.06 10 0.4 25 — — — — 486 500
P-30% 2.87a 14 0.8 22 8.8 15 31 22 1096 895
C-0 3.06 — — 26 — — — — 231 265 [56]
C-30% 2.82a 5 2 20 3.3 7.5 23 42 852 821 [55]
a
Taylor factors for P-30% and C-30% are estimated from corresponding EBSD maps. Considering the weak initial
textures, the Taylor factors for the undeformed samples are chosen to be 3.06. Details about the dislocation density
estimation can be found in the Supplementary materials S5.

sonable to assume the same strengthening effect for twin bound-

Fig. 11. Idealized sketches illustrating the deformed microstructure of printed sam-
ples and conventionally manufactured samples. (a) C-30%, showing the twin–matrix
(T–M) lamellar structure as well as the Taylor lattice structure consisting of domain
boundaries (DB) and microbands (MB); (b) P-30%, showing the T–M lamellar struc-
ture (double sets of twins) and the rolling–induced cells in the structure delineated
by cellular dislocation boundaries (CeDB).
aries as that of grain boundaries for 316 L stainless steel. For P-30%,
the calculation overestimates the yield strength by 22%, which may
be partly caused by using the average spacing of the inhomoge-
neous T–M lamellae. There is a higher fraction of T–M lamellae of
smaller average HAB spacing in P-30% compared to C-30%, indicat-
ing a stronger effect of twinning in strengthening P-30% than in
C-30%. However, further investigations are needed to evaluate the
strengthening contribution of the inhomogeneous T–M lamellae in
3D printed samples more precisely.
5. Conclusion

The present study investigates the microstructural evolution of

tor; α is a constant; G is the shear modulus; SV is the area per unit
volume of low angle dislocation boundaries (taken to be 2 times
the number of intersections per unit length PL , assuming random
distribution of low angle dislocation boundaries); θ is the aver-
age misorientation angle of low angle dislocation boundaries; b is
the Burgers vector; ρ0 is the density of loose dislocations; K1 is
the Hall-Petch constant; D is the grain size (spacing of high angle
boundaries). The constants for 316 L are shown in Table 1.
For C-30% and P-30% containing a mixture of twin–matrix (T–
M) lamellar structures and dislocation structures, as shown in
Fig. 11, the flow stress σ (ε ) is given by the rule of mixture [45,54]:
 √
σ (ε ) = (1 − fT −M )(σ0 + Mα G 1.5SV θ b + ρ0 b2 + K1 / D )
   tion twinning process in terms of the initiation and propaga-
KT −M
+ fT −M σ0 + √ + Mα Gb ρ0T −M
2λ
where fT −M is the volume fraction of T–M lamellae, ρ0T −M is the
dislocation density in T–M lamellae, λ is the average spacing of
T–M lamellar structure, and KT −M is a constant representing the
strengthening effect of HABs in T–M lamellar structure, taken to
be the same as K1 , i.e., assuming the strengthening effect of twin
boundaries is identical to that of grain boundaries.
In the above analysis, residual stresses are considered to not
have a significant effect on the yield strength as the residual
stresses are balanced on the sample scale. Table 2 shows the mi-
crostructural parameters quantified from EBSD and TEM images, as
well as the calculated and experimentally measured yield strength.
For C-0, only grain boundary strengthening is considered; for P-0,
both grain boundary and dislocation boundaries are considered but
the strengthening contribution from loose dislocations is ignored.
The calculated yield strength σcal is almost identical to the experi-
mental results σexp for the cases of P-0 and C-0. For C-30%, there is
only 3% difference between σcal and σexp , indicating that it is rea-
3D printed stainless steel 316 L during cold rolling and compares
to that of conventionally manufactured counterparts. The strength-
ening contributions of different microstructural features are ana-
lyzed; the yield strength is calculated based on microstructural pa-
rameters and compared to experimental results. The main conclu-
sions are as follows:
(1) The pre-existing dislocation boundaries suppress long-range
planar glide of dislocations, and therefore the Taylor lattice
structure, which is commonly observed in conventionally
manufactured 316 L, does not develop in 3D printed sam-
ples. Instead, rolling-induced dislocation cells of an average
size of 125 nm form inside the cellular structure.
(2) The pre-existing dislocation structure can pivot the deforma-
(2) tion, leading to thinner and denser twins in 3D printed sam-
ples. This is because the pre-existing dislocation structure
facilitates deformation twinning by providing twinning par-
tial dislocations. Yet, this structure also acts as an obstacle—
either as a repelling force between dislocations or by form-
ing Lomer-Cottrell locks.
(3) The 3D printed samples have a higher work hardening rate
compared to the conventionally manufactured ones at the
same stress level. Strength calculation suggests that the thin-
ner and denser deformation twins, whose formation is fa-
cilitated by the pre-existing dislocation structure, contribute
significantly to the high strength of 3D printed samples after
deformation.
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared to
influence the work reported in this paper.

8
C. Zhang, D. Juul Jensen and T. Yu
Acknowledgment
The main part of this work was carried out within M4D project
supported by the European Research Council (ERC) under the Eu-
ropean Union’s Horizon 2020 research and innovation program
(Grant agreement No. 788567). The tensile testing part of the work,
which was added based on comments from the reviewers, was car-
ried out in the RePowder project funded by the Danish Council
for Independent Research (Grant No. 9041-00335B). CZ further ac-
knowledges the financial support of the China Scholarship Council
(CSC) (N0. 201706120026).
Supplementary materials
Supplementary material associated with this article can be
found, in the online version, at doi:10.1016/j.actamat.2022.118481.
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