Experimental Characterization of Stainless Steel 316L Alloy Fabricated With Combined Powder Bed Fusion and Directed Energy Deposition

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Welding in the World (2021) 65:1373–1388

https://doi.org/10.1007/s40194-021-01117-z

RESEARCH PAPER

Experimental characterization of stainless steel 316L alloy fabricated


with combined powder bed fusion and directed energy deposition
Kumaran M 1 & Senthilkumar V 1

Received: 18 August 2020 / Accepted: 23 March 2021 / Published online: 5 April 2021
# International Institute of Welding 2021

Abstract
Powder bed fusion (PBF) is an additive manufacturing (AM) technique commonly used to manufacture metallic components.
External geometry of parts printed by PBF process can be extended by regular processes, namely, laser cladding and spraying
powder metal. But these methods have disadvantages such as increased heat-affected zone (HAZ) and extended deficiencies like
cracks and pores, whereas samples produced with directed energy deposition (DED) exhibited strong metallurgical bonding and
has reduced HAZ due to least dilution. The present work investigates the properties of stainless steel 316L (SS316L) sandwich
structure built by combining PBF and DED process. The external geometry of the SS316L samples built by PBF was extended by
using DED technique. Metallurgical and mechanical characteristics of DED extended PBF samples were studied. Tensile
properties such as percentage elongation and tensile strength were compared for PBF, DED, and SWS (DED extended PBF).
It was found that the yield stress for the DED samples, PBF samples, and SWS samples is in the range of 486 MPa, 564 MPa, and
401 MPa. Moreover, the average hardness of the interface portion is found to be 220.5 HV and it is higher than the hardness
observed in the PBF and DED regions.

Keywords Additive manufacturing . Stainless steel 316L . Sandwich structures . Powder bed fusion . Directed energy deposition

Nomenclature PR Powder feed rate (g/min)


AM Additive manufacturing SS Scanning speed (mm/min)
PBF Powder bed fusion P Laser power (W)
DED Directed energy deposition E Energy density (J/mm2)
SS316L Stainless steel 316L
HAZ Heat-affected zone
FESEM Field emission scanning electron microscope
EBSD Electron back scattered diagram
XRD X-ray powder diffraction
1 Introduction
SWS Sandwich structures
Metal-based AM process [1, 2] gained attention due to bene-
EDAX Energy-dispersive X-ray spectrometer
fits in the manufacture of complex structural components
DMLS Direct metal laser sintering
which are hard to produce through conventional processes like
DMD Direct metal deposition
casting, forging, and rolling. ASTM categorised metal-based
AM techniques into DED [3–5] and PBF [6–8]. DED can
manufacture components by depositing the metal powder in
Recommended for publication by Commission I - Additive a specific location. PBF manufactures 3D parts by selectively
Manufacturing, Surfacing, and Thermal Cutting irradiating high energy onto a bed where the metal powder is
spread [9]. Presently, the DED process is mostly used for
* Senthilkumar V repair work [10, 11], but literature indicates a trend where it
vskumar@nitt.edu
can be used to develop and extend an already built PBF spec-
1 imens [12, 13]. Cheng-Xu Ren et al. and Zhanqi Liu et al. [14,
Department of Production Engineering, National Institute of
Technology Tiruchirappalli, Tiruchirappalli, Tamil Nadu 620015, 15] have used the DED technique for developing sandwich
India structures from similar or dissimilar materials.
1374 Weld World (2021) 65:1373–1388

While metallic products produced by AM have amazing sandwich structure fabricated by combining PBF and DED.
mechanical characteristics [16], it has to be investigated for Further, a comparison between the mechanical and micro-
adopting in industries. If the structure which already exists structural properties of PBF, DED, and SWS specimens are
needs to be enlarged for an application, it has to be modified made.
for reuse instead of being replaced. Welding, wire arc addi-
tive, laser cladding, metallizing, and brazing are traditional
ways to extend such products. However, due to their suscep- 2 Experimental procedure
tibility to produce pores, cracks, and wider HAZ, more ad-
vanced laser melting techniques like DED are suggested. 2.1 Materials and experimental setup for PBF and DED
DED can reduce the HAZ of the interface region to create a
perfect structure. In DED the contact area is less which ac- SS316L spherical granules in a diameter range of 5–45 μm
counts for the reduction in the heat-affected zone. Moreover, and 50–150 μm were used for PBF and DED processes, re-
in DED process, the chances of powder agglomeration, poros- spectively, in this study. The chemical composition of the
ity, surface defects, and dilution rates with previously depos- above powders is provided in Table 1.
ited layer are very less. Thus, the parts produced by DED Figures 1a and 2a show the morphology of SS316L pow-
would offer high geometrical fidelity as compared to the wire der as observed in FESEM. Powder particles are spherical but
arc additive manufacturing. It is also possible to make com- have varied sizes. Histograms for particle size distribution are
plex shapes by adjusting the laser nozzle accurately. In previ- shown in Figures 1b and 2b indicating an average particle
ous studies, the surface of DED manufactured components diameter of 22 μm and 80 μm, respectively, for the PBF and
were studied by fabricating components at different powder DED processes. Energy-dispersive X-ray spectrometer
feed rate, laser power, and scanning speed. Surfaces on the (EDAX) results shown in Figs. 1c and 2c reveal that samples
border of the deposited layers were observed, and equiaxed of chemical compositions meet the standard values of
microstructures were found at the top and bottom of the de- SS316L. Hall flow test (ASTM B213) results ensured powder
posited region [17]. Differences were identified in mechanical particles flowability as a continuous and consistent powder
and microstructure characteristics by adjusting the deposition flow rate is essential as it affects the AM process [21].
distance amongst layers during DED manufacturing, which Spherical-shaped particles make powder flow quickly through
also proved the mechanical properties of the components the deposition nozzle orifice.
manufactured by DED conventionally. SS316L substrate for the present study was fabricated
Till now, laser melting deposition (DED) studies used tra- by direct metal laser sintering (DMLS) (EOS M280,
ditionally manufactured base components for rebuilding. Germany). DMLS process (PBF) uses a continuous wave
Several other researchers results have shown [11, 12, 18], over Yb (Ytterbium) fibre laser with a laser power of 400 W;
the PBF developed component additional new surfaces were 1100 nm wavelength with multi-mode and 500-μm diam-
built using DED process. This kind of developing a new geo- eter. The three-axis laser CNC control device with the
metrical surface over the existing component. Since two dif- process software (PSW) controlled the build process,
ferent processes were involved in fabrication, the tensile spec- while other systems measured and controlled printing of
imens of PBF and DED sandwiched zones were opted for the components. Substrates were built with a scanning speed
tensile study to identify the weakest zone undergoing fracture. of 900 mm/s, 200-W laser power, 100-μm hatching pitch
Further, fractography results elucidate the nature of fracture. with 400-μm layer thickness and 0.2-mm laser diameter
The present study focused on SS316L [19], a material com- in a completely an inert ambience without infiltration of
monly used in industrial applications as it has excellent corro- atmospheric gases. The above parameters were the same
sion resistance, high-temperature strength and weldability. as those used for virgin powder which yielded the least
Most of the researchers have studied the mechanical proper- porosity with superior mechanical properties [22].
ties of the PBF fabricated SS316L specimens by varying pro- Direct metal deposition (DMD) machine used in the pres-
cess parameters such as powder feed rate, laser power, and ent work (POM-DMD 105D, USA) is shown in Fig. 3a, and
scanning speed [20]. However, the present investigation aims the images of the building up of extended part on the initial
to study the mechanical and microstructural properties of PBF substrate is shown in Fig. 3b–c. The DMD machine had a

Table 1 Chemical composition


of SS316L [% by weight] Element/material Fe Cr Ni Mo Si Mn C N P S

PBF (5 to 45 μm) 68.34 16.62 10.57 2.11 0.60 1.58 0.030 0.10 0.035 0.020
DED (50 to 150 μm) 68.66 16.99 10.59 2.00 0.2 1.4 0.01 0.10 0.024 0.007
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Fig. 1 PBF SS316L powder: (a) FESEM morphology, (b) histogram of particle size distribution, and (c) EDAX results

Fig. 2 DED SS316L powder: (a) FESEM morphology, (b) histogram of particle size distribution, and (c) EDAX results

Fig. 3 (a) DMD metal additive


manufacturing machine, (b) ready
to start DED process above the
PBF subtract, and (c) during DED
process
1376 Weld World (2021) 65:1373–1388

Table 2 DED process parameters


by the Taguchi method Sample Parameters Energy density
(J/mm2)
Laser power Scanning Powder feed
(W) speed (mm/min) rate (g/min)

a 400 300 2 133.333


b 400 500 3 80
c 400 700 4 57.142
d 600 300 3 200
e 600 500 4 120
f 600 700 2 85.714
g 800 300 4 266.666
h 800 500 2 160
i 800 700 3 114.285

five-axis CNC deposition platform controlled by DMD-CAM considered the main process parameters which in a specific
path generation software, including a laser system with 1 kW combination influenced the geometric, metallurgical, and me-
of fibre coupling. The machine had four powder hoppers to chanical properties of the material deposited. Optimal setting
supply powder, and powder nozzles to deliver processing gas of these parameters is vital to produce geometrically accurate
and powder. Argon was used to inject the powder to prevent samples with good mechanical properties.
oxidation during manufacturing. An optical device was
mounted on the head where the powder was fed. A 0.6-mm
diameter nozzle supplied the laser beam and powder. The 2.2 Effect of DED process parameters by the Taguchi
distance between the nozzles from the substrate’s surface method
was 15 mm. A high-power laser beam penetrates the powder
on the substrate’s surface forming a melt pool. The melt pool Multi-layer deposition experiments were conducted to estab-
rapidly solidifies after the beam had passed, forming the de- lish the best condition by varying process parameters like
position bead. During manufacturing, the parameters are re- powder feed rate (PR) scanning speed (SS) and laser power
peated to form a layer. Powder feed rate, layer thickness, laser (P). L9 orthogonal array used for conducting experiments [3]
scanning speed, hatching pitch, and laser power are is shown in Table 2.

Fig. 4 Micro-hardness test results


of samples fabricated with
varying process parameters
Weld World (2021) 65:1373–1388 1377

Fig. 5 Microscopic image of DED deposition samples developed with varying process parameters (sample (a–i))

Trial DED experiments were conducted according to L9 Figure 5 shows the microstructural images of the SS316L
array to deposit samples of 4 mm high, 5 mm length, and samples processed through DED under different process
5 mm width above the substrate. Samples hardness after pro- conditions and varied laser power of 400, 600, and 800 W.
duction was tested with a Vickers micro-hardness tester [4]. Figure 5a–c are the result of 400 W laser power where aver-
Hardness results are indicated in Fig. 4. Optical images of all 9 age micro-hardness is about 180.5, 176.3, and 157.6 HV,
samples are shown in Fig. 5a–i. The same were used to char- respectively. It is observed that the micro-hardness values
acterize the melt pool and porosity. decreased gradually, the reason being that a moderate

Fig. 6 (a) PBF substrate and (b) DED extended specimen (SWS)
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Fig. 7 (a) and (b) Configuration of the tensile specimens

increase in the porosity level of the unmelted region leads to processing conditions of 600-W laser power, 500 mm/min
low density reflecting a reduction in hardness values. scanning speed, and powder feed rate of 4 g/min were select-
Figure 5d–f shows the result of 600-W laser power where ed as optimal conditions. The above DED processing param-
average micro-hardness is about 217.5, 225.4, and 218.6 eters were used to build up material on PBF substrates.
HV, respectively. This is much attributed to higher powder
density as very low porosity was observed in this condition. 2.3 Production of sandwiched structure specimen
There was no indication of unmelted powder which resulted
in relatively higher hardness values. Moreover, the refined Figure 6a–b show the AM SS316L substrate prepared using
grain induced during laser processing by rapid heating and PBF and an extended specimen with DED process. The PBF
cooling improved micro-hardness. Figure 5g–i show the re- substrate prepared was of 15 mm height (Z-axis, upright
sult of 800-W laser power where average micro-hardness position) and it was extended by a similar length by resorting
was about 204.5, 209.7, and 208.2 HV, respectively. to the DED process in order to produce SWS. Excessively
Compared to earlier process conditions, hardness was re- accumulated material was removed from the SWS, and the
duced further. The outcome resulted in good density simul- samples were sliced with a wire cut EDM machine to create
taneously revealing un-melted powders between layers [23]. tensile samples in the build direction in accordance with
Based on the microstructural and harness analysis results, ASTM (E8) standard [23] as shown in Fig. 7a–b. To compare

Fig. 8 (a) Scale dimensions of tensile specimen and (b) different AM tensile specimens
Weld World (2021) 65:1373–1388 1379

the tensile properties of SWS samples, entire parts produced Figure 10 describes the FESEM micrograph of the ex-
with PBF and DED were cut along the build direction and the tended portion. Figure 10 a–b are magnified (×500 and
same is shown in Fig. 8. ×1000) images of the PBF and DED bonding structure
A uniaxial tester (Tinius Olsen H50KL) of 50-kN capacity specimens, respectively. All microstructural images show
was used for the tensile test. The fractured surfaces of all three three distinct regions, namely, HAZ, substrate, and dilu-
test samples (PBF, DED, and SWS) were characterized. tion. The dilution zone is where the substrate is supposed
Micro-hardness measurements were carried out along the to be melted when the first layer of DED is deposited,
building direction of samples. The SWS sample was polished wherein mixing of molten powder with the substrate oc-
for microstructural study using a silicon carbide polishing curs in the melt pool. Very fine HAZ of 3 μm thickness is
sheet; etching solution (HCl:1, H2O:3, HNO3:6) with 3V seen clearly in the samples immediately below the dilution
and 2Amperes current [18]. Macro- and micro-structures were area suggesting highly localized heating and rapid cooling
studied using optical microscope and FESEM images. EDAX that occurred during the DED process. Figure 10 c–d show
results were used for the element analysis of all test samples. the PBF substrate and DED extended component’s micro-
structure. Columnar grains and epitaxial grain growth were
observed in both PBF substrate and DED area along the
build direction. Figure 10 e shows the DED sample’s mi-
3 Results and discussion crostructure near the substrate’s interface with no signifi-
cant difference in the expanded DED region. Figure 10 f
3.1 Microstructure shows the columnar grain growth followed by equiaxed
grain growth very nearer to the deposited area between
Microstructural images and the corresponding magnified im- PBF and DED (magnification—×2500). Generally, solidi-
ages of extended SWS specimens are shown in Fig. 9. Regions fication rates have low correspondence with columnar
A and B indicated in the microstructure are areas produced with structures nearer to the track’s surface [18]. As compared
PBF and DED processes, respectively. The interfacial region is to the top layers, bottom most layers would undergo faster
indicated as C [12, 13]. Fabricated samples show no pores or heat dissipation due to the substrate attachment which can
cracks in the SWS suggesting excellent metallurgical bonding result in directional solidification. The grains tend to grow
between substrate and the extended region. in a direction opposite to the direction of heat dissipation.

Fig. 9 Microstructural images of extended SWS specimens (a) PBF portion, (b) DED portion, and (c) Interface region (SWS portion)
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Fig. 10 FESEM micrographs of the (a) extended zones, (b) interface portion, (c) PBF portion, (d) DED portion, (e) and (f) near the interface

From inverse pole figure, it is evident that grains of the Figure 11 a–b show microstructures of the DED specimen
DED fabricated surface were grown in opposite direction taken along the 1st, 2nd, and 3rd layers. The first, second and
of the PBF sample. In DED process, the columnar to third layers of deposition indicate that grain in each bead
equiaxed transition will be high due to the least dilution changes from columnar structure to an equiaxed structure.
rates. It is due to the fact that thermal gradient (G) to the Due to sudden heat dissipation through the interface, some
grain growth velocity (R) ratio (G/R) ratio is too low in grains have grown epitaxially in the columnar portion. The
DED process; thus, high fractional equiaxed grains were existence of equiaxed grains suggests that homogeneous nu-
spotted out, whereas in PBF sample, more fraction of cleation occurs during the process through quick solidifica-
coarser columnar dendrites were found due to the wider tion. Figure 11 c shows that the bonding interface layer thick-
HAZ because of dilution effects. Therefore, columnar to ness is 3 μm including the HAZ and dilution portions, an
equiaxed transition was hindered in PBF sample [24]. observation similar to that reported elsewhere [18].
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Fig. 11 (a) and (b) FESEM micrographs of the interface portion and (c) bonded interface layer’s thickness

Figure 12 shows EBSD maps and the pole figure of an Differences in composition are due to the nature of the pro-
as-built AM SWS specimen along the build direction. In cess. In laser melt deposition, fast cooling speed resulted in
the PBF portion, the as-built specimen has a relatively uniform morphology for each bead leading to a minor segre-
smaller grain size. Most grain boundaries indicate very gation [5, 18].
high misorientation angles. The DED portion noted from
the inverse pole figure maps reveals that microstructure 3.2 Micro-hardness
does not exist in cell form but rather as larger grain size.
Most grain boundaries revealed very low misorientation Figure 14a–b show micro-hardness values for the PBF and
angles. Due to the laser melting deposition’s rapid DED specimens and that of the interface of the SWS spec-
cooling, the columnar grain of the DED component was imen. Average hardness of PBF, DED, and the interface
shaped vertically in the building direction. In the as-built region were 209.7 HV, 218.6 HV, and 220.5 HV, respec-
specimen, the equiaxed cellular crystal structure was dis- tively (deposition direction). Finer equiaxed grains corre-
tributed in orientations (111), (001), and (101). spond to the DED process and coarser columnar grains
Comparing EBSD maps of the as-built specimen’s DED corresponds to the PBF process. Therefore, the micro-
region with that of the PBF region, green and red regions hardness values of DED and PBF samples are completely
increased and blue regions decreased. This means different. It has been widely reported that overlapping
strengthening the orientation (101) and (001), and the layers due to dilution effects lead to agglomerated grains.
weakening of orientation (111) [22, 23]. Thus, there was a drop in micro-hardness at the overlap-
A scanning line of the interface between the PBF and DED ping layers. In DED process, the micro-hardness anisotro-
samples was conducted to investigate the difference in the py was very minimum. It is because HAZ- of DED-
extended specimens alloying elements (Z-axis, building direc- fabricated component is very less, and finer equiaxed
tion). As shown in Fig. 13a, the laser melting deposition of the grains were spotted out. Finer grains offered superior
PBF and DED portions had different compositions. micro-hardness according to the Hall-Petch empirical phe-
Figure 13b–d show each element being distributed uniformly. nomenon [25]. Also, composition difference observed in
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Fig. 12 EBSD inverse pole figure of the as-built specimen: (a) Inverse pole figure map, (b) IQ map, (c) boundary map, (d) grain size distribution, and (e)
misorientation angle distribution of the SWS sample (red: [001]; blue: [111]; green: [101])

the EDAX results as shown in Fig. 13a–d revealed that the was checked using ferritoscope [24]. Also Fig. 14 reveals
interface region has more iron content than the individual the average hardness of the interface portion to be 220.5
DED- and PBF-treated surfaces. From the inverse pole HV which is more than the hardness observed in the PBF
figure, it could be concluded that DED samples undergo and DED regions [23].
faster cooling rate as compared to the PBF sample.
Materials such as SS316L have low Cr/Ni ratio. For such 3.3 X-ray diffraction (XRD)
metals the on increasing cooling rate the ferrite content will
be less. Similarly, DED processed sample showed less fer- XRD images were used to evaluate the phase constituents of
rite content as compared to the PBF sample. The accuracy SS316L powder particles, PBF, DED, and the interface
Weld World (2021) 65:1373–1388 1383

Fig. 13 (a) EDAX results of the SWS specimen, (b) PBF portion, (c) DED portion, and (d) interface portion

regions. XRD images of PBF, DED, and interface regions of 3.4 Tensile properties
SWS along with particles used for the above two processes are
shown in Fig. 15. Diffraction peaks obtained with coordina- Figure 16 shows the tensile test results of the PBF, DED, and
tion planes in the 2θ values were 43.62° (111), 50.81° (200), SWS specimens. When individual PBF and DED specimens
and 74.70° (220) indicating that SS316L powders, PBF, DED, were compared before extending, yield stress of the PBF spec-
and SWS specimens have FCC (face-centred cube) austenite imen was 564 MPa, at a total elongation of 45.5%, with ulti-
phase with no ferrite phase [5, 6]. mate stress being 675 MPa. Yield stress of the DED specimen

Fig. 14 (a) Different processes in micro-hardness values. (b)Average micro-hardness of PBF, DED, and SWS
1384 Weld World (2021) 65:1373–1388

Fig. 15 XRD spectrum of


SS316L

was 486 MPa, at a total elongation of 48.7%, and ultimate extended process (SWS) tensile test specimens revealed that
stress 676 MPa. On the other hand, the PBF sample showed yield stress of the SWS specimen was 401 MPa, with a total
a yield stress 78 MPa higher than that of the DED specimen. elongation of 47.1% and ultimate stress of 557 MPa. The
The PBF specimen’s elongation was 3.2% less when com- strength of all three samples was almost equal, and increase
pared to the DED specimen. Ultimate stress of the PBF and in elongation in the SWS specimen was 1.6% as compared to
DED samples were almost similar. Further, higher strain hard- the PBF specimen [3, 18]. Figure 17 shows the comparisons
ening was seen in the DED samples. These variations were of ultimate stress, yield stress, and total elongation of the three
due to the characteristics of the laser melting deposition and different specimens tested [26].
the resulting microstructural variation. In contrast to the DED Figure 18 shows the macro-images of PBF, DED, and
specimen, the PBF specimen produced coarse grains, and SWS tensile samples after fracture during tensile loading.
hence, the DED specimen tends to have high strength and PBF and DED specimens fractured in the middle of the
elongation. As a result, dislocation movement was difficult region, while the SWS specimens fractured above the cen-
while the material’s strength increased. The results of the tre of the extended zone. Specifically, strength and

Fig. 16 Engineering stress-strain


curve of the deposited SS316L
Weld World (2021) 65:1373–1388 1385

Fig. 17 Comparisons of the (a) ultimate stress, (b) yield stress, and (c) total elongation

elongation of the SWS sample decreased by 1.6% com-


pared to that of the PBF and DED specimens. Ultimate
stress of the SWS sample was almost the same as that of
the other two specimens. Initiation of crack occurred due
to repeated cycles of melting and solidification during
DED laser powder deposition. The crack in the specimen
was propagated and easily ruptured due to subsequent
loading along with stress concentration [9, 18].
Figure 19 a–c show the FESEM fractograph along the ex-
tended, heat-affected, and substrate regions of the fractured
specimens. Dimples were observed in the PBF and DED
structures. Dimples were seen in the DED portion of the
SWS structure. HAZ showed simultaneous dimples, quasi-
cleavage, and a ductile and brittle fracture behaviour, respec-
tively, which lead to a low percentage of elongation in the
specimens [5, 10].
As the number of melting-cooling cycles increased with
each laser transfer, thermal stress near the interface increased.
As the extended region’s height increased, the number of de-
position layers was also more thereby increasing chances of
further extension. Mechanical properties of the extended sam-
Fig. 18 Macro-images of PBF, DED, and SWS Specimens, (i, ii, and iii, ples deteriorated a little due to this. Nevertheless, this research
respectively) after tensile testing revealed that when extended height was increased, there was
1386 Weld World (2021) 65:1373–1388

Fig. 19 FESEM fractograph of the fractured specimens: (a) PBF tensile specimen, (b) DED tensile specimen, and (c) SWS tensile specimen

no significant change between the mechanical properties be- fabricated by extending the substrate produced by the PBF
fore and after the extension. In such a method, the extension process using laser metal deposition (DED). The SWS speci-
process of DED proved suitable for components of SS316L. men was evaluated for its tensile test results, XRD, and mi-
crostructural studies. The following conclusions are drawn
from the studies:
4 Conclusions
(1) Multilayer DED specimens were fabricated with differ-
The mechanical and microstructural characteristics of laser ent process parameters and optimal scanning speed.
deposition of SS316L powder in the DED process were stud- Optimizing key variables such as powder feed rate and
ied to optimize process parameters. SWS specimens were laser power the fine grain configuration could be tailored.
Weld World (2021) 65:1373–1388 1387

The fine grain configuration without porosities could re- 5. Guo P, Zou B, Huang C, Gao H (2017) Study on microstructure,
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Technology Institute (CMTI), Department of Additive Manufacturing, the quasi-static compression behavior of multilayer aluminum foam
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