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International Journal of Lightweight Materials and Manufacture 5 (2022) 384e396

Contents lists available at ScienceDirect

International Journal of Lightweight Materials and Manufacture

journal homepage: www.keaipublishing.com/ijlmm

Original Article

Biomedical porous scaffold fabrication using additive manufacturing


technique: Porosity, surface roughness and process parameters
optimization
Palash Mondal a, Apurba Das b, *, Adil Wazeer c, Amit Karmakar a
a
Department of Mechanical Engineering, Jadavpur University, Kolkata, 700032, India
b
Aerospace Engineering and Applied Mechanics Department, Indian Institute of Engineering Science and Technology-Shibpur, Howrah, 711103, India
c
School of Laser Science and Engineering, Jadavpur University, Kolkata, 700032, India

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

Article history: Titanium is a most common and best biocompatible material. The demand and application of Ti alloy is
Received 3 January 2022 increasing rapidly in orthopedics for clinical operations. The porous structures have been designed for
Received in revised form bone tissue engineering or orthopedic applications due to its moderate Young's modulus, excellent
16 April 2022
compressive strength, biocompatibility and sufficient space for cell accommodation. The porous scaffolds
Accepted 21 April 2022
Available online 29 April 2022
with individual complex internal and external shape can be manufactured by additive manufacturing
(AM) processes especially selective laser melting (SLM), both of these have great importance for repairing
of large sectional bone defects. This advantage makes the SLM process one of the most competitive AM
Keywords:
Tie6Ale4V
processes used in the biomedical fields. Seven different Tie6Ale4V porous scaffolds (Diamond, Grid,
Additive manufacturing Cross, Vinties, Tesseract, Star and Octet) of 15 mm cube with 65% porosity were designed using Rhino 6
Selective laser melting software and fabricated through SLM using Tie6Ale4V powders. This work mainly focused on porous
Porous scaffolds scaffolds design and manufacturing by AM particularly SLM, can able to produce scaffolds of nanoscale
3D printing grains because of its higher heating rate and lower holding time. But this process generally results
insufficient compaction where desired function is not achieved. The scaffolds manufactured by SLM have
relatively high accuracy of pore structure and low mechanical strength. Grid type structure exhibits
lower surface roughness value and better manufacturing ability where error percentage of porosity is
lower than the other scaffolds.
The process parameters employed in the study like laser power, scanning speed, hatch distancing and
layer thickness are the most significant factors that influence the defect behaviour and morphology of
the SLM-fabricated samples. Porosity percentage and surface roughness of the scaffold palys a vital role
on its desired functions. While the porosity percentage are also effected by input process parameters
resulting the variation on effective elastic modulus. The increase in scanning speed leads to elevation of
the cooling rate, which results in a finer microstructure. On the other hand, with lower scanning speeds,
coarse microstructure is observed.
© 2022 The Authors. Publishing services by Elsevier B.V. on behalf of KeAi Communications Co. Ltd. This
is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/
4.0/).

1. Introduction extension and also to keep dilatation as stent grafts while bio-
medical implants should have moderate elasticity, excellent
Mechanical properties play the centre role for materials where strength, fatigue resistance and toughness. For replacement of
higher plasticity and adequate rigidity is required to permit joints and dental implants wear may occur serious damage on the
material surface and debris into the body. For that case hard and
fatigue resistant materials are generally used. Stainless steels are
widely used in biomedical fields due to its corrosion resistance,
* Corresponding author. mechanical strength and relatively low price [1e3]. The most
E-mail address: [email protected] (A. Das).
commonly stainless steel is 316L which is widely used to make pins,
Peer review under responsibility of Editorial Board of International Journal of
Lightweight Materials and Manufacture. plates, rods or screws, intramedullary nails incases of craniofacial

https://doi.org/10.1016/j.ijlmm.2022.04.005
2588-8404/© 2022 The Authors. Publishing services by Elsevier B.V. on behalf of KeAi Communications Co. Ltd. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
P. Mondal, A. Das, A. Wazeer et al. International Journal of Lightweight Materials and Manufacture 5 (2022) 384e396

and bone fixation as described by Disegiand Eschbach [4]. Besides the best methods for manufacturing of porous scaffolds [18]. Before
that, CoeCr alloys, have been successfully employed in orthodontic additive manufacturing process, generally a 3D scaffold is modelled
applications and artificial joints due to their excellent hardness and with proper dimensions through Rhino 6 software. Then the 3D
wear resistance as replacement of knee and hip prosthesis [2,3]. model is cut into a number of 2D pieces before converting to stereo
Titanium alloys, because of its outstanding Young's modulus and lithography (STL) files containing information in details of 2D slice
corrosive resistance, high specific strength and stiffness and excel- by slicing algorithm. Then an AM machine performs along the
lent biocompatibility, are widely used in orthopedic applications, necessary tool path depending on these STL files to build of 2D layers
which are more similar to bone than other alloys [5e7]. But dense Ti directly and every layer is built over the another layer to make a 3D
alloys have greater elastic modulus (E ¼ 112 GPa) whereas bone part. This manufacturing process of adding a layer over the another
tissues (E ¼ 4e30 GPa) [4]. Different elastic modulus causes the load is known as AM. Recently, around the world most of the researchers
redistribution all over the implant, loosening of implant and are applying these AM techniques to fabricate porous implants in
autogenous fracture of bone, is called stress shielding [8]. This stress bone repair. Poukens [19] used AM to manufacture porous implants
shielding effect is the primary cause of instability at the interface and that was successfully implanted into a patient body in due
between hard tissues and usual metallic implants and to overcome course. Jardini et al. [20] customize porous scaffolds to overcome
these issues porous networks have been introduced in the dense large cranial defects using AM technique. AM porous titanium is
materials [10]. Porous scaffolds can able to prevent osteonecrosis, used to amputate a heel bone for elderly patient. Due to these suc-
osteo-genesis irregularities successfully round the implant. In cesses the AM techniques have surely a promising future in bone
addition, the inter-connected porous scaffolds are useful for differ- tissue repair. In this work seven types porous scaffolds are modelled
entiation, adhesion and proliferation of bone tissues [11]. with 65% porosity and these models are fabricated by selective laser
Bone tissue can able for biological rebuilding of the mature bone melting method. The only parametric details and manufacturing
tissue absorption by osteoclasts and new bone for next generation process of porous scaffolds are discussed in this work. The theo-
by osteoblasts through a dynamic process [12,13]. However, the retical and actual porosity after preparing the samples are measured
body normally cannot make self-repairing fully when a large and compared.
segmental bone defect takes place and it exceeds the critical size of
10 mm [14]. In this situation, an external interference is necessary to 2. Material selection and methods
support for self-repairing in the form of making bridges on the bone
defect place. So, bone grafts are widely used in clinical operations to 2.1. Powder material
support for curing of these type of defects. Data collected from dis-
ease control centers exhibit that the bone is a secondary graft tissue Tie6Ale4V powders (Supplied by EOS GmbH, Germany) of
and over 20 lakhs surgical operations employing bone grafts in each nearly spherical in shape with smooth surface and a particle
year [15]. Besides, autografts are taken from patient itself and are diameter below 90 mm were used as a raw material to fabricate the
measured as the gold standard for repairing of bone but it is very porous scaffolds as shown in Fig. 1(a) and Fig. 1(b) shows the dis-
limited in size. In addition to this, autografts are harvested certainly tribution of particle size obtained by the method of laser diffraction
because at the time of additional surgical trauma that is associated at according to Coulter principal. Visual observation of this powder is
the donor site with a severe risk of morbidity. carried out using optical microscope Olympus BX41 or GX51 (EOS,
As of now, the maximum metallic implants were manufactured Finland) to investigate powder monolayer and mounted, polished
by traditional processes which include forging, hot rolling, invest- samples. The analysis of particle size distribution and powder
ment casting and machining [16]. But a new technology has been properties in this work are shown in Table 1 and Table 2
developed named additive manufacturing (AM) since last 30 years. respectively.
According to ASTM [17], AM is defined as the “process of joining Based on the chemical composition (shown in Table 3), the
materials to make objects from 3D model data, usually layer upon scaffolds were manufactured and it is found that the percentage of
layer”. The AM technique, particularly selective laser melting (SLM) iron, carbon, hydrogen, oxygen and nitrogen are very low in Ti64
with excellent individual external shape control is known as one of powder.

Fig. 1. (a) Morphological micrograph of Tie6Ale4V raw powder for SLM Manufacturing; (b) Particle size distribution of Tie6Ale4V powder.

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P. Mondal, A. Das, A. Wazeer et al. International Journal of Lightweight Materials and Manufacture 5 (2022) 384e396

Table 1 2.2. Design and fabrication of porous scaffolds


Particle size distribution analysis.

Size Characteristics Test Method Result (mm) In the present work seven different types of porous 3D scaffolds
d10 Laser Diffraction 29.48
(Diamond, Grid, Cross, Vinties, Tesseract, Star and Octet) of Ti alloy
d50 47.05 (as shown in Fig. 2) were designed by Rhino 6 software of 15 mm
d90 71.92 cubes with 65% porosity. A specific density of 4.41 gm/cm3 and
relative density of 100% (approx.) for Ti64 was used.
In this work, the models are heat treated for 2 h at 800  C with a
Table 2
heating rate of 5  C/min and finally cooled at room temperature in a
Powder property analysis. furnace in the presence of an inert gas (argon) environment. The
oxygen content was kept below 8 ppm in the build chamber and
Property Test Method Result
the scanning strategy is illustrated in Fig. 3.
Apparent density ASTMB212 2.42 gm/cm3 All the seven samples are fabricated by a SLM machine (Model:
Tap density ASTMB527 2.9 gm/cm3
Density ISO3369 4.41 gm/cm3
EOSINT M280-400W) with the following input process parameters
Water content Karl Fischer titration 25.6 ppm for TI-6AL-4V materials as shown in Table 4.

2.3. Additive manufacturing (AM)


Table 3
Chemical composition of Tie6Ale4V powder used in this work.
On the basis of metal powder AM processes, models are man-
Element Ti Al V Fe C H O N ufactured by adding one layer upon another with the help of a laser
(wt%) (wt%) (wt%) (ppm) (ppm) (ppm) (ppm) (ppm)
or electron beam by melting powders. In all AM processes, at first
Mass Balance 5.5e6.75 3.5e4.5 <3000 <800 <150 <2000 <500 3D models are designed by Rhino 6 software. These 3D models are

Fig. 2. Computer model of Tie6Ale4V porous scaffolds: (a) Diamond (b) Cross (c) Grid (d) Vinties (e) Tesseract (f) Star and (g) Octet.

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P. Mondal, A. Das, A. Wazeer et al. International Journal of Lightweight Materials and Manufacture 5 (2022) 384e396

additive manufacturing. This technology, which is still in its early


stages of development, has been used in the biomedical sector to
fabricate bone supports and replacements. The technology was first
studied for the manufacturing of jaw and bone implants in the field
of dentistry and orthopedics.
A typical SLM machine and process are illustrated in Figs. 4 and
5. The SLM process consists of metal powders as raw material, a
laser, beam focusing arrangement, feeder mechanism and build
plate. In the process of SLM, 3D metal parts are manufactured by
fusion of fine metallic powders using the energy from a laser beam
basically an ytterbium fiber laser of wavelength ranging from 1.06
to 1.08 mm, and operated at 1 kW as shown in Figs. 2 and 3. A layer
of fine metallic powder is used to the building platform by a blade,
and the powders melt by laser beam into the 2D cross sections in an
inert environment, which can be controlled as required. The
galvanometer controls the beam focus and the F-theta lens governs
the movement of the beam. Then lower the building platform to
Fig. 3. SLM manufacturing process. apply another layer. Until the building of 3D part is completed this
process continues. The thickness of layer may vary from 15 to
150 mm.
Table 4 SLM technique depends on parameters like material type,
Input process parameters used in SLM process for Tie6Ale4V.
scaning, laser source and atmospheric conditions. For the selected
Parameters Value materials, a parametric study was performed to optimize the entire
Type of Laser Ytterbium Fibre Laser process including the density of parts because the mechanical
Shape of Spot Spherical characteristics of the components is greatly affected by the
Scan Speed (SS) 1000e1500 mm/Sec porosity. Primarily four parameters have been selected during the
Diameter of Particle (PD) >90 mm
process for experimentation namely laser power, thickness of layer,
Hatch Distance (HD) 0.02e0.14 mm
Power of Laser (LP) 225e475 W scanning speed and hatch distancing. The energy, supplied by the
Diameter of Laser (LD) 80 mm laser beam, is determined by Ref. [21]:
Density (r) 4.41 g/cm3
Thickness of Layer (LT) 60 mm
Initial Temp. of Bed (Ti) 35  C
Scan Angle of Rotation (q) 67 Pl
200mm  200mm  200mm
Ed ¼ (1)
Building Space ðvs htÞ
Environment Maintained Inert
Scan Path “X" & Rotational
where Ed ¼ energy density, Pl ¼ laser power, vs ¼ scan speed,
h ¼ hatch distancing and t ¼ layer thickness.
The energy density describes the amount of energy applied per
then converted into STL files. The STL model slices it into a number unit volume of the powder material. The variation of the input
of 2D layers by slicing algorithm. The additive technologies have process parameters changes the volume energy density and also
numerous applications in the field of biomedical including tissue affects the density and quality of the fabricated parts. The above
generation, organoids, implants, anatomical models and custom- equation shows the higher energies causes higher melting and
ized prosthetics fabrication. There are various AM techniques but decreases with increase in layer thickness, scanning speed and
only few of them have the potential of fabricating the porous hatch distancing. A high energy density is required to achieve high
structures with complex internal and external gemoetries by densification by completely moltening the powders. The energy
varying different parameters. The AM approaches that are widely input for the SLM process is also influenced by the process pa-
employed in the biomedical sector are laser powder bed fusion rameters and can be described as [22]:
(LPBF) or selective laser melting (SLM), electron beam melting
(EBM), directed energy deposition (DED) and laser metal deposi-
tion (LMD). 4Pl
Ei ¼   (2)
The AM techniques have developed most of the industrial sec- pd2l vs
tors like biomedical, automotive, aerospace and jewellery to offer
more advantages to the producers and customers. AM technologies
where Ei ¼ energy input, Pl ¼ laser power, dl ¼ diameter of laser
have most relevant advantages including the product custom-
beam and vs ¼ scan speed.
ization, tooling costs reduction, consumption of waste and energy,
Another is linear energy density (LED) that can also be used to
on demand manufacturing possibility and supply of new chain
calculate the energy input of powder material as [23]:
approaches. AM technologies offer to make complex shape of or-
thopedic products such as functionally graded parts, novel shapes
and hollow structures to improve the compatibility of implants, Pl
patient wellness within short time and excellent corrosion resis- LED ¼ (3)
vs
tance to improve tissue ingrowth, adhesion and cell migration.
where Pl ¼ laser power and vs ¼ scan speed.
2.4. Selective laser melting (SLM) process for Tie6Ale4V The porosity percentage (P) depends on the process parameters,
energy density (Ed), scanning speed (v), laser power (Pl) and hatch
In 2002 the selective laser melting (SLM) was introduced as one distancing (h) and the relationship between them can be expressed
of the methods for producing complicated parts using metal as:
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P. Mondal, A. Das, A. Wazeer et al. International Journal of Lightweight Materials and Manufacture 5 (2022) 384e396

Fig. 4. Eos direct metal laser sintering machine (model: EOSINT-M280).

Fig. 5. Schematic of typical Selective Laser Melting (SLM) process for fabrication of Ti64 porous lattice structures using SLM system EOSINT-M280.

! A part fabricated by the SLM process when compared with


Ed vs h2 traditional process like cast and forged have excellent mechanical
P¼f (4)
pl properties, have good grain refinement characteristics, reduction of
phases egregation size, solid solubility and chemical homogeneity.
The building rate is directly proportional to the scanning speed The melting characteristic of metallic powders is affected directly
(vs), hatch distancing (h) and layer thickness (t). The available laser by the process parameters like scan line spacing, laser power and
power limits the scanning speed and layer thickness. The building scan speed. Therefore, the process parameters are controlled
rate of SLM process is determined by the product of scanning speed, carefully to fabricate superior quality biomedical devices. Computer
hatch distancing and layer thickness and can be expressed as: layout and actual picture of manufactured samples on the machine
bed are shown in Fig. 6 and Fig. 7.
Vb ¼ vs ht (5) SLM is used to print complicated geometries or lightweight
structures in a variety of sectors, including aerospace, automotive,
where Vb is the building rate (mm3/s). In the present study, the and biomedical. Printed components may have thin walls, deep
scanning speed, hatch distancing and layer thickness are consid- voids, and concealed channels, making it a viable method for
ered as 1250 mm/s, 0.12 mm and 60 mm respectively for which the making porous scaffolds. Although higher temperature gradients
maximum building rate is 9.0 mm3/s while the relative density might cause residual stress, this can be avoided by properly post-
achieved was at least 99.98%. heating the component.

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P. Mondal, A. Das, A. Wazeer et al. International Journal of Lightweight Materials and Manufacture 5 (2022) 384e396

Fig. 6. Computer layout of modelson the machine bed.

Fig. 7. Actual picture of the manufactured samples on machine bed.

2.5. Effect and optimization of process parameters

The characteristics of AM porous scaffolds are influenced by


various input process parameters during the SLM process. The
improvement of density is the main concern for the porous scaffolds
manufactured by SLM. Fully dense struts are also desirable in porous
scaffolds. Furthermore, because of the severe non-equilibrium
condition during SLM, a unique microstructure has been observed.
This is due to the rapid cooling of the melt pool during the process,
which causes the variation of mechanical properties.
It has been observed from Fig. 8 that the effects of process pa-
rameters (such as laser power, scan speed, and hatch distance) on
relative density of Tie6Ale4V samples made using SLM and the
scanning speed has also a significant effect on relative density. Now
an optimization study is required to determine the ideal processing
parameters for achieving the desired density during fabrication by
SLM. The goal is to achieve maximum density with no restrictions
on process parameters. Table 5 shows the optimal set of parameters
are 340 W power, 1250 mm/s scanning speed, 0.12 mm powder Fig. 8. Variation of relative density (%) with volume energy density (J/mm3).

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P. Mondal, A. Das, A. Wazeer et al. International Journal of Lightweight Materials and Manufacture 5 (2022) 384e396

Table 5 proliferation and differentiation [24]. To get the required rough-


Optimized process parameters and build system of Tie6Ale4V using ness, the implant surface can be improved through acid etching,
SLM.
sandblasting and plasma spraying [25]. The metal powder based
Parameters Result processes are able to produce implants of desired surface rough-
Scan Speed (SS) 1250 mm/Sec ness in osteointegration. During SLM process, number of Ti parti-
Power of Laser (LP) 340 W cles of spherical shape are bonded partially with the porous walls.
Hatch Distance (HD) 0.12 mm Then the specimens are heat treated at 800  C in an argon atmo-
Thickness of Layer (LT) 60 mm
sphere and then micro cavities are formed on the walls, and further
promoted for interlocking to the adjacent tissues while implanted
into the human body. Biemond et al. [26] reported a comparative
layer thickness, XeY inter-layer stagger scanning and 0.06 mm analysis on the quality of surfaces of trabecular implant manufac-
hatching space. The powder layer thickness also influences the tured by SLM and EBM. The specimens were manufactured by SLM
surface roughness and microstructure of the porous scaffolds. and EBM techniques demonstrates different morphological char-
During the SLM process, the high layer thickness increases the acteristics and surface roughness: In the specimens fabricated by
surface roughness of the scaffolds. EBM process, the individual granules were clearly visible, whereas
Aside from the machining input process parameters, there are a in the specimens fabricated by SLM process, the surface rough-
number of scaffold design factors that have a significant effect on nesses were flattened than the surfaces by EBM. This difference of
mechanical and biological properties. Pore morphology, unit cell accuracy between these two approaches is responsible for the
shape, and strut thickness are factors to consider. From Fig. 9, it is variation in porosity as well as post treatment surfaces.
observed that the process parameters are the most important fac- It is found that the SEM image of the Tie6Ale4V powder which
tors which affect the porosity of SLM-fabricated samples. is nearly spherical in shape with a smooth surface as shown Fig. 1.
The roughness value (Ra) of the prepared samples is measured by a
2.6. Surface roughness and morphology Talysurf surface roughness tester (MITUTOYO SJ-210) as shown in
Fig. 10 and is presented in Table 6. Lower surface roughness is
Surface roughness and energy, may affect the implant and bone observed for the grid type of sample. Based on literature [27] if Ra is
tissue and can also prevent osteoblastic cell adhesion, growth, less than 25 mm, the surface roughness has a positive effect and

Fig. 9. Effect of input process parameters of Tie6Ale4V scaffolds during SLM.

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P. Mondal, A. Das, A. Wazeer et al. International Journal of Lightweight Materials and Manufacture 5 (2022) 384e396

when Ra is greater than 57 mm, it will have a negative effect. The Table 6
surface treatment of porous implants is not necessary up to 25 mm Roughness value (Ra) of prepared samples.

and if the roughness value exceeds 25 mm then surface treatment is Sample Type Roughness value (Ra) in mm
needed. Based on this, the samples are required to surface treat- Sample1 Sample2
ment. The grid type sample shows the minimum surface roughness
Diamond 46.2 49.6
while the diamond type sample exhibits higher surface roughness
Cross 43.7 41.8
value. Grid 23.2 21.6
It is observed in different studies concerning whichever to make Vinties 27.7 29.8
the following surface treatments are mostly contradictory. The re- Tesseract 31.3 30.6
Star 33.8 35.1
sults on osteoblasts stated by Ponader et al. [27] to the surface
Octet 29.3 31.6
roughness of implants by EBM that the arithmetic average value of
the absolute roughness values (Ra) plays a vital role in the differ-
entiation and as well as proliferation of human osteoblasts.
displaced water gives the theoretical volume of the scaffold with
porosity as shown in Fig. 11. The difference in actual volume of the
2.7. Porosity measurement of manufactured scaffolds sample without porosity and the theoretical volume of the scaffold
gives the porosity data. The measured porosity value for each
The porosity of the prepared samples are measured using the sample is shown in Table 7.
density principle. Each samples were immersed in water in a The porosity of Tie6Ale4V scaffolds can be determined as:
measuring cylinder which is minutely graduated and the volume of  
Wp
P¼ 1 x100% (6)
Wd

where, P ¼ Porosity, Wp ¼ Weight of the porous sample and


Wd ¼ Weight of the densed samples.
The percentage of error for the grid type of sample is lowest
while diamod type shows maximum porosity difference as shown
in Fig. 12. The grid type sample could show greater resemblance
with minimum deviation.

2.8. Optimization study of the porosity results

The DOE has been carried using the Taguchi analysis method.
The results of the porosity of the different samples were obtained
and further these results were studied for the optimization
employing the Taguchi method utilizing the Mitnitab software.
Optimization study of the Porosity percentage versus scan speed
(mm/sec), hatch distance (mm), laser power (W) is perfomed. Re-
sponses and graphs of Mean and Signal to Noise ratios were ob-
tained. Two level study of each sample is done and results are
recorded. Fig. 13 represents the graphs of the Mean effects plots for
means for each sample. Fig. 14 represents the graphs of the Mean
effects plots for SN ratios for each sample.

3. Mechanical properties

The microstructure of the materials improves the mechanical


properties which are strongly affected by AM process. In this pro-
cess the scaffolds are manufactured by a set of repeated heating and
cooling during the layer upon layer production of materials.
Particularly, initial particles go through by quick heating to melting
point by absorbing energy from a source of laser or electron beam.
The melting portion of the material solidifies quickly to develope of
coarse grained microstructures after scanning by the energy source.
To process of the next layers, the remaining portion of the material
is uncovered for repeated heating. This compound thermal cycle
causing the metastable microstructures and structural phases
which can also be changed in the part volume. Depending on the
heat transfer the depth of melt portion can be varied in different
AM processes. Generally, in LMD, the heat transfer involves with
convection to the shield gas, conduction to the substrate and built
material. But in SLM processes, a powder bed is present all over the
part causing limits the heat conduction, reduces the gas flow rate
and the contribution of convection. Generally, EBM manufactures
Fig. 10. Talysurf surface roughness tester (Mitutoyo SJ-210). Tie6Ale4V parts of coarser microstructure compared with the
391
P. Mondal, A. Das, A. Wazeer et al. International Journal of Lightweight Materials and Manufacture 5 (2022) 384e396

Fig. 11. Porosity measurement of fabricated porous scaffolds by measuring cylinders.

Table 7 cycles which can be easily modified to get better mechanical properties
Measured porosity of the prepared samples. by thermal post processing. Generally, the selection of treatment op-
SampleType Theoretical porosity Measured porosity tions also can influence strongly the grain size and orientation, phase
Sample 1 Sample 2
evolutions, precipitation, densification and stress relief.
The relationship between the modulus of elasticity and porosity
Diamond 65% 62.7% 62.4%
percentage can be approximately determined by the simplified
Cross 65% 63.4% 63.8%
Grid 65% 64.2% 64.5% expression as [28]:
Vinties 65% 64.4% 64.6%
Tesseract 65% 63.2% 63.9% Ep ¼ Es ð1  PÞ2 (7)
Star 65% 64.5% 64.0%
Octet 65% 62.7% 62.7%
where Ep ¼ effective Young's modulus of porous material, Es ¼
Young's modulus of dense or solid material and P ¼ porosity.
The both elastic modulus and relative elastic modulus (elastic
modulus ratio of porous scaffold to solid scaffold) are decreasing
with increase in porosity % (shown in Fig. 13). From Eq. (7), the
effective Young's modulus can be calculated and is equal to
13.72 GPa (considering the Young's modulus of solid Ti alloy as
112 GPa and porosity as 65%), which is similar to human bones
(E ¼ 4e30 GPa).

4. Results and discussion

Tie6Ale4V powders with particle diameter below 90 mm are


used as a raw material to fabricate the porous scaffolds. Then based
on the internal procedures, the visual observation of powder is done
using optical microscope Olympus BX41 or GX51 (EOS, Finland) to
investigate powder monolayer. Tie6Ale4V powder is almost
Fig. 12. Percentage of error in porosity of different prepared samples. spherical in shape with smooth surface and contains very less
amount of iron, carbon, hydrogen, oxygen and nitrogen. Seven
numbers of porous 3D scaffolds (Diamond, Grid, Cross, Vinties,
products by SLM or LMD at low cooling rates. On the other hand, a Tesseract, Star and Octet) of 15 mm cube were designed by Rhino 6
very high degree of undercooling is only due to higher cooling rate software using Tie6Ale4V powders with 65% porosity and a specific
more than 104K/s and very high thermal gradient in SLM and LMD density of 4.41 gm/cm3. All the samples have been manufactured by
processes. selective laser melting (SLM) machine EOSINT M280-400W, has
The mechanical properties of Tie6Ale4V alloys by SLM process will optimized by 60 mm thickness of layer, a laser power of 340W and the
be determined in ISO17025 accredited laboratory according to ISO diameter of laser beam of the laser source is 100 mm. During SLM
6892-1 or ASTM E8. During AM process, to develope the metastable manufacturing, the laser is rotated through 67 between the two
microstructures and phases due to quick solidification and thermal adjacent layers. Porous scaffolds were heat treated at 800  C for 2 h
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P. Mondal, A. Das, A. Wazeer et al. International Journal of Lightweight Materials and Manufacture 5 (2022) 384e396

Fig. 13. (a) The effect of porosity on elastic modulus (b) The effect of porosity on relative elastic modulus.

in an inert atmosphere, and at last cooled at room temperature in a spheroidization occurs, resulting in poor bonding between the
furnace to improve the mechanical properties. layers and un-melted powder particles, resulting in a low relative
Titanium alloys, because of its outstanding Young's modulus and density. And when the ratio of laser power and scan speed is too
corrosive resistance, high specific strength and stiffness and high, the melting track depth is increased, the height is small,
excellent biocompatibility, are widely used in orthopedic applica- making it difficult to form, and the phenomena of element evap-
tions. But dense Ti alloys have greater elastic modulus of about oration and ablation is easy to occur during the forming process,
112 GPa whereas bone tissues have 4e30 GPa. Generally higher resulting in density reduction. Increase in hatch distance resulting
strength and stiffness and lower ductility (E ¼ 112 GPa, yield partial melting of the powder and inclusion. As a result, only the
strength ¼ 945 MPa, UTS ¼ 1050 MPa and ε ¼ 14%) [29,30] are appropriate ratio of laser power to scan speed and hatch distance
found for Tie6Ale4V materials in SLM process. To avoid stress may achieve higher relative density and are optimized at 0.272 J-
shielding the implants should be similar to human bones mm and 0.12 mm respectively.
(E ¼ 4e30 GPa) followed by mechanical, biological and chemical Microstructure influences the mechanical properties of the
properties. Due to this the porous network has been introduced in scaffolds. Therefore, different scan speed are characterized to get
to the dense materials to get desired mechanical properties by better microstructure of the fabricated samples by SLM. The
controlling porosity. And it has been observed from Fig. 11 that microstructure of the samples by SLM process are quite different
when the porosity is about 60e70%, the Ti porous scaffolds give the rather than the samples manufactured by other traditional tech-
similar value of human bones. Then the samples are required to niques, such as welding, casting. An increase in scan speed leads to
surface treatment as surface roughness affects the implants. The an increase in cooling rate, which leads to a finer microstructure. As
grid types ample shows the minimum surface roughness while the a result of the slower scan speed, the microstructure is coarser.
diamond type sample exhibits higher surface roughness value. The
other variants show the values in between. Based on the porosity
measurement of the prepared samples, the porosity error per- 5. Industrial scope of present work
centage for the grid type of sample is lowest while diamond type
shows maximum. The grid type sample has minimum deviation of Depending on the production and creation feasibility for
porosity. reproducing patient organs, tissues and implants the AM processes
The density of the scaffolds play a key role to optimize the are extensively used in the field of medical applications. AM tech-
process parameters since it has a direct impact on the mechanical, nologies also allow to make the complex replication of structure of
physical and also biological properties of the part. The relationship nerves, bones and muscles and as a result the surgical interventions
between relative density and the product of three factors is char- get easier in implants without any severe risk. The AM, reduces the
acterized as volume energy density (VED) and expressed as Equa- span of tooling operations and wastage of materials (up to 75%) as it
tion No. (1). Fig. 3 shows the relationship between relative density is too faster and cheaper in production of medical devices, has
and VED. The relative density first increased, then decreased as VED excellent mechanical strengths as compared with traditional
increased. The relative density reaches its highest value, which is manufacturing processes. Wohlers [31] stated that over 100,000
close to 100%, when the VED is around 40 J/mm3. From Fig. 9, it is acetabular implants were manufactured by AM processes and
observed that with increase in porosity percentage the energy among them about 50,000 were successfully implanted in patient's
density, scanning speed and hatch distancing also increasing and body in recent years. This data proves that the demand and interest
the laser power decreases with increase in porosity percentage of Tie6Ale4V alloys by AM in biomedical applications have grown
obtained from Equation No. (4). When the ratio of laser power and drastically in different industrial sectors due to its excellent me-
scan speed is too low, the melting channel depth is reduced and chanical properties as shown inTable 8 [29,30].

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P. Mondal, A. Das, A. Wazeer et al. International Journal of Lightweight Materials and Manufacture 5 (2022) 384e396

Fig. 14. Mean effects Plots for SN Ratios for each sample (a) Diamond (b) Cross (c) Grid (d) Vinties (e) Tesseract (f) Star (g) Octet.

394
P. Mondal, A. Das, A. Wazeer et al. International Journal of Lightweight Materials and Manufacture 5 (2022) 384e396

Table 8 Funding
Mechanical properties of dense Tie6Ale4V alloy.

Property Method Result The author(s) received no financial support for the research,
Yield strength ISO 6892-1 945 MPa
authorship, and/or publication of this article.
Tensile strength Or ASTM E8 1200 MPa
Compressive Strength 1050 MPa Conflicts of interest
Elastic modulus, E 112 GPa
Elongation, A 14%
The authors declare that there is no conflicts of interest.
Reduction of area, Z 47%

Acknowledgements
6. Conclusion
The authors acknowledge Khishimoto-Inaba Laboratory of
Tokyo Institute of Technology for providing guidance during
In this study seven different types of porous scaffolds with in-
preparation of this work.
dividual complex internal and external porous structures (having
theoretical porosity of 65%) are modelled and manufactured by
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