Materials Science & Engineering A 804 (2021) 140759

Contents lists available at ScienceDirect

Materials Science & Engineering A

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

Effects of morphological characteristics on the mechanical behavior of 3D

printed ordered pore topological Fe scaffold
Dipesh Kumar Mishra, Pulak Mohan Pandey *
Department of Mechanical Engineering, Indian Institute of Technology, Delhi, India

A R T I C L E I N F O A B S T R A C T

Keywords: Ordered pore topological structures (OPTS) provide various features such as biodegradability, cell proliferation,
Micro-extrusion based 3D printing and matching mechanical property for bone tissue repair and ingrowth at a single platform. Therefore, the de­
Compressive behavior mand for OPTS have shown an unexpected rise in the field of biomedical due to trauma, deformity, and aging
Ordered pore
population, etc. Moreover, these OPTS have found widespread applications in the form of biodegradable ma­
Strut size
Biodegradable materials
terials. Hence, the interest in pure iron as a biodegradable material has been growing rapidly due to its better
mechanical properties. However, the slow degradation rate of iron is a major challenge. Therefore, iron-based
OPTS have been advantageous to limit the slow degradation rate. In the current work, OPTS have been manu­
factured using the novel fabrication technique comprising of micro-extrusion-based 3D printing and pressureless
microwave sintering. Two dissimilar types of unit cell shapes viz. hexagonal and cubic were chosen to fabricate
the OPTS with three different strut sizes such as1.0, 1.25, and 1.5 mm. The variation in dimensions of OPTS was
found to be less with respect to the designed CAD model. Moreover, the OPTS dimensions were compared to
other conventional metal printing techniques such as indirect solid free form manufacturing technique. The
compressive behavior of fabricated OPTS inferred Young’s modulus, ultimate compressive strength, and energy
absorption capacity of 136–257 MPa, 11–67.3 MPa, and 2–15 MPa, respectively. Moreover, the compressive
mechanical behavior of fabricated OPTS was found to be in line with the Gibson-Ashby model. A discussion was
performed to compare the results of the present study with the prior work and it was evident that properties of
manufactured OPTS were obtained to lie in the desirable range, and it can be considered as for the development
of orthopedic applications.

1. Introduction fluid transport. Additionally, 3D (three-dimensional) printed inter­

connected porous scaffolds were best matched for biological applica­
With a progressively busy lifestyle, tumors, obesity, accidents, and tions like bone regeneration. The addition of porous features in the
an aging population, the requirement for bone reconstruction has un­ fabricated scaffolds was famously known as foam [5].
expectedly increased. The self-repair feature of bone may avoid minor The materials utilized for fabricating the foam can be classified into
damage. However, it requires an external intervention on major damage composite, polymer, glass, metallic and ceramic-based materials.
[1]. Thus, the demand for external intervention triggered the advance­ Generally, the metallic based foam is used as a permanent bone
ment of bone tissue engineering. The growth of biomaterials for bone replacement for high load bearing characteristic in the human body. The
tissue engineering is essential to fulfill the booming needed for bone effect of long-term stability of the metallic foam in the human body
reconstruction [2]. However, the bone has a complex architecture of under reactive in-vivo condition possesses additional risk like another
nature and possesses diverse and dynamic mechanical properties. The surgical requirement. As a result, the study of biodegradable materials
Young’s modulus of human bone (of cancellous type) lies between the have been widely explored in recent decades [6]. The biodegradable
ranges of 0.1 to 5 GPa [2]. For bone reconstruction, biomaterials should materials belong to the category of biomaterial that completely dissolves
have compatible strength with the human bone matrix. Recent studies inside the human body as bone regenerates [7]. Frequently used
[3,4] reported that the addition of porous features within the artificial biodegradable materials in biomedical applications are glass, polymer,
bone scaffold offers better osseointegration property and supports body metallic, and ceramic-based. Apart from metallic based materials, others

* Corresponding author.
E-mail addresses: [email protected] (D.K. Mishra), [email protected] (P.M. Pandey).

https://doi.org/10.1016/j.msea.2021.140759
Received 31 October 2020; Received in revised form 29 December 2020; Accepted 4 January 2021
Available online 8 January 2021
0921-5093/© 2021 Published by Elsevier B.V.
D.K. Mishra and P.M. Pandey Materials Science & Engineering A 804 (2021) 140759

have limited use in bone tissue engineering due to lower mechanical disadvantages such as incurring high fabrication costs due to expensive
strength to support bone regeneration. In order to meet the current and 3D printer. In order to reduce the manufacturing cost, Sharma and
fast-growing demand for supporting bone reconstruction, metallic based Pandey [30] have proposed the seven-step fabrication route. These
biodegradable implants are being used successfully [8,9]. In the biode­ seven-steps consisted of designing an intent porous template using 3D
gradable metallic materials, the most explored metals are magnesium printing (Stereolithography). Further, a designed template was used to
(Mg), iron (Fe), and zinc (Zn) [6,8]. A majority of the researchers [1,6] fabricate OPTS after heating in a microwave sintering furnace. The
have reported that the Mg-based implant exhibited excellent mechanical massive processing steps (seven-steps) may obsolete the fabrication
and biocompatible properties similar to the human bone matrix. How­ process. Therefore, extrusion-based 3D printing can be adopted to print
ever, the fast degradation rate of the Mg-based bio implant owing to the or fabricate the OPTS of metallic parts with small processing steps.
hydrogen formation limits its application for more massive lifespan Furthermore, extrusion-based 3D printing is an ink-based dispensing
bio-implants [1,6,10]. Therefore, it appears to be suitable for those system assembled with an automatic arm that extrudes the uninter­
bio-implants whose lifespan is mainly around 6–12 months [6,11]. rupted flow of filament via the micro-size nozzle. The filament is
Contrarily, Zn-based bio-implants have an ideal degradation rate; deposited as per the path guided by CAD software [31,32]. In the recent
however, their inferior mechanical properties make these unsuitable for study, the random porous iron structures were manufactured using an
biodegradable scaffold applications [8,12]. amalgamation of extrusion-based 3D printing and conventional sinter­
On the other hand, Fe-based implants have better mechanical ing processes [33]. However, conventional sintering makes the
properties and they offer sufficient strength for high bearing load [13]. It manufacturing process time-consuming with increased
is pertinent to mention that, Fe is a mandatory element found in the energy-consumption and also induces weak mechanical properties [34,
human body for providing better transportation of oxygen and proper 35].
functioning of various enzymes. However, the slow degradation rate of From the literature review, it could be inferred that ordered pores
iron in the physiological environment limits its bone implant applica­ have desirable biological and mechanical properties in relation to
tions [6]. The alloying with elements like manganese, phosphorus, sil­ random pore distribution. Therefore, it is required to develop an ordered
ver, and palladium resulted in a substantial increase in the degradation pore topological Fe structure (OPTFS) with different unit cell structures.
rate of the iron [9,14,15]. Moreover, a higher Young’s modulus of Fe as Moreover, the limited experimental attempts [8,29] studied the effect of
compared to human bone raised the chance of stress-shielding, and different morphological characteristics on the mechanical behavior of
which may further cause reduced bone regeneration [16]. In a recent OPTFS. However, due to difficulties in the processing or microwave
study [1], it was revealed that the fabrication of interconnected porous sintering of Fe, very few studies have focused on developing reliable and
structures could found to be a promising solution for reducing higher safe methods for fabricating OPTFS. Therefore, the aim of this study to
Young’s modulus and slower degradation rate. Additionally, using the fabricate ordered pore topological structures (OPTS) using novel
proper designing of the porosity (i.e., pores) of the scaffolds could meet micro-extrusion-based 3D printing and pressureless microwave sinter­
with the strength and Young’s modulus required for bone reconstruction ing. Further, the compressive mechanical behavior of fabricated
[6,8]. Further, the degradation products of porous iron scaffolds do not Fe-based OPTS were evaluated by varying the unit cells such as cubic
produce a poisonous impact on the various living enzymes. Moreover, and hexagonal with different strut thicknesses. Morphological charac­
the increased exposed surface area due to the porous structure was terizations of developed Fe based OPTS with different unit cells were
found to another cause to increases the degradation rate with no evo­ performed using optical microscopy images. Additionally, the
lution of hydrogen bubbles [17–19]. Gibson-Ashby model [6] was used to compare and form a relationship
The researchers [6,20,21] have reported various fabrication routes with the mechanical properties obtained from the static compressive
to develop a porous iron structure. However, all these fabrication routes load.
are not fit for creating a porous structure with a small pore size required
for a better osseointegration property [22]. Plunk and Dhunad [21] 2. Materials and method
reported the technique for fabricating the lamellar type iron foam
through the directional freeze casting of iron oxide slurry in an atmo­ 2.1. Materials
sphere of hydrogen. Quadbeck et al. [20] fabricated the porous iron by
infusing polyurethane foam through a slurry of iron. Another way for In order to fabricate the biodegradable metallic scaffold, carbonyl
successfully manufacturing the porous iron based on powder metallurgy iron particles (CIPs), polylactic acid (PLA), and solvent mixture were
route was reported by Capek et al. [6] wherein ammonium carbonate used in the present work. CIPs with an average particle size of 2.0 μm
used as a space holder. It was informed [6] that the properties of the and having 99.5% purity were procured from BASF, Germany. Scanning
manufactured scaffolds were found compatible with the human bone electron microscope (SEM) image of CIPs can be inferred from Fig. 1 (a).
matrix. However, the techniques mentioned above were associated with In order to determine the particle size distribution (PSD) of different
major demerits like the generation of random pore design. This random sizes of CIPs, an image processing tool (Image J) was utilized to perform
pore design has resulted in undesirable mechanical properties like the measurement and it can be seen from Fig. 1 (b). It is evident from the
bending and twisting of the fabricated strut and reduction in effective SEM image (Fig. 1 (a)) that the morphology of iron particles was
stress. Further, it slows down the degradation rate and nutrients trans­
port through biodegradable scaffolds [8,23]. In order to cater to this
problem, the researchers have proposed the ordered pore topology
structure of metal foam [6,8]. The different manufacturing techniques
were used to fabricate the ordered pore topology structures (OPTS) of
metal foam. Recently, it was found that 3D metal printing has emerged
as a better fabrication route to develop OPTS [24–26]. Selective electron
beam melting [25,27] and selective laser melting [27,28] techniques
were widely used for the fabrication of metallic OPTS. Currently, the
fabrication of porous Fe-based OPTS using direct metal printing (DMP)
was reported by Y. Li et al. [29]. The resulted property of fabricated
OPTS was found compatible with the biodegradation profile and offered
relatively similar properties required for bone reconstruction [29].
Nevertheless, the methodology mentioned above exhibited major Fig. 1. (a) SEM image, and (b) particle size distribution of CIPs.

2
D.K. Mishra and P.M. Pandey Materials Science & Engineering A 804 (2021) 140759

observed to be nearly spherical. PLA (Polylactic acid, 4060D grade,

supplier Nature works) was used as a polymer-based binder in this work.
Moreover, the solution mixture used for developing the metallic-based
polymeric ink consisted of dichloromethane (DCM), 2-butoxyethanol,
and dibutyl phthalate (supplier Thermo-fisher). These inks were made
ready by amalgamation with the right proportion of CIPs with the binder
solution in a solvent mixture.

2.2. Method

The schematic diagram of steps involved in a developed methodol­

ogy for the fabrication of OPTS has been presented in Fig. 2. The method
started with the designing of the Computer-Aided Design (CAD) model
using designing based software. The technique used for fabricating the
OPTS was pronounced in the authors prior work [36]. With the aid of the
developed CAD model, 3D printing of the green body of OPTS was
fabricated using the prepared metallic-based polymeric ink. The
metal-based polymeric inks were formulated using the vortex and ul­
trasonic bath mixing of CIPs and PLA with a ratio of 7.5:2:1 by a mass
mixture solution (of DCM, 2-butoxyethanol, and dibutyl phthalate).
The solution of CIPs was made ready by adding 8.1 g of a solvent
mixture (DCM + 2-butoxyethanol + dibutyl phthalate) in each volume
of the metal powder. The other binder solution was prepared by indi­
vidually dissolving PLA in DCM in the proportion 1 : 15. Subsequently,
the dissolved solution of the binder was assorted with CIPs solution
through an ultrasonic bath (mixing for 60 min). Further, it was simul­
taneously concentrated by evaporation of DCM, yielding a uniform ink
mixture without amalgamation. Moreover, the image of prepared ink
can be seen in Fig. 3 (a). Additionally, the detailed study of the rheo­
logical behavior of prepared ink can be referred from the authors pre­
vious work [37,38]. The prepared metallic-based polymeric inks were
then utilized to fabricate the green body of OPTS with the assistance of
micro extrusion-based 3D printing. The optimum printing parameters
used for printing the OPTS were determined by central composite design
and the Genetic Algorithm [37]. These printing parameters consisted of
94.3 wt.% of Fe loading, 0.1 mmof layer thickness and 73 % of infill
density [37]. Thereafter, heating of 3D printed OPTS was done in a
microwave sintering furnace (supplier Enerzi microwave systems). This
heating was performed at an optimized set of sintering parameters
which were obtained in the prior study performed by Mishra and Pandey Fig. 3. (a) Image of prepared ink, (b) Heating cycle used for fabricating the
[38]. The heating cycle at an optimized set of sintering parameters, used OPTS [37].

for fabricating the OPTS has been displayed in Fig. 3. In the present
work, the two-stage heating cycle was used to fabricate the OPTS. In the
first stage, the thermal debinding of binders was performed. As a result,
binders were completely removed from the green body of the printed
scaffold [38]. Thereafter, the next stage of isothermal heating resulted in
the strengthening of the fabricated part. The pressureless microwave
sintering of OPTS resulted in the densification of the powder particles
thereby eliminating the use of a compact die. Thus, using the developed
methodology complex-shaped can easily be fabricated without the use of
a compact die.
After that, the surfaces of fabricated OPTS was cleaned using sand­
blasting followed by ultrasonication in ethanol for 30 min. For surface
finishing, the glass bead powder within the average size of 75 μm was
utilized. The two dissimilar unit cells such as cubic and hexagonal were
chosen for the manufacturing of OPTS. Aforementioned types of unit
cells were selected in the current objective because of higher compres­
sive and specific strength and better morphological properties [8,39].
Therefore, the efficacy of the developed process was analyzed by per­
forming mechanical testing and morphological characterization. The
different level of porosity was attained in cubic, and hexagonal based
OPTS by changing its strut thickness while keeping the overall volume
kept constant. The different strut thicknesses were kept as 1.0 mm, 1.25
mm, and 1.5 mm. For cubic based unit cell, ordered pore topological
Fig. 2. Steps involved in fabrication of OPTS.

3
D.K. Mishra and P.M. Pandey Materials Science & Engineering A 804 (2021) 140759

structure (C-OPTS) has designed a strut thickness of 1 mm (C-1), 1.25

Ds
mm (C-1.25), and 1.5 mm (C-1.5), respectively. In parallel for the RD = (1)
D
hexagonal-based unit cell ordered pore topological structure (H-OPTS)
has designed strut thickness of 1 mm (H-1), 1.25 mm (H-1.25), and where Ds is the density of sintered Fe scaffold, and D is the density of
1.5 mm (H-1.5), respectively. In order to avoid the boundary effects, the iron (7.87 g/cm3 ). The relative density was used to calculate the porosity
seven repeated cells were designed in the fabricated OPTS along to the (P) of the fabricated scaffold as per equation (2):
direction of loading [5]. The illustration of the CAD model, 3D printed
green part, and fabricated part of OPTS with different pore architecture P = (1 − RD ) × 100% (2)
and strut sizes are depicted in Fig. 4. The different pore morphology of the fabricated OPTS was examined
by a Dino-lite optical camera. The strut thickness and pore size were
measured, after calibrating the microscope as per the standard scale. The
2.3. Structure characterization measurements were done at three different locations of strut thickness
and pore size of each fabricated OPTS using the microscope interface.
The density of the porous iron scaffolds was determined as per the The average of these three values and their standard deviations (SD)
ASTM B962-13 standard [40]. The measurements were repeated three were determined and matched with a designed CAD model to check the
times and its average value has been reported. Subsequently, the density variation in dimensions.
of the scaffolds was further used to calculate the relative density (RD)
using equation (1): 2.4. Compression testing

The testing of samples was performed as per the ISO 13314 standard
[41]. Three samples were fabricated for each cubic based unit cell and
hexagonal based unit cell with different strut thickness respectively. In
pertinent to this, triplicate compression tests were conducted at each
condition and its average value was reported. The overall size of the
sample used for fabricating the C-OPTS and H-OPTS were 22 × 22 ×
22 mm3 and 25 × 21 × 25 mm3 , respectively. Moreover, the compression
testing of the fabricated OPTS samples was executed at a Universal
Testing Machine (Instron 5582) with a constant crosshead speed of
1mm/min. The compressive engineering stress-strain curves were
plotted after utilizing the calculated value of the applied load and its
corresponding displacement of fabricated samples. Compressive prop­
erties like yield strength (σy ) and Young’s modulus (EC ) were deter­
mined by utilizing the 0.2 % offset method and using the slope of the
elastic portion of the compressive stress-strain diagram. Moreover, the
ultimate compressive stress (UCS) was considered as the first local
maximum compressive stress and plateau stress (σpl ) was measured
using considering the average value of compressive stress between 20 to
40 % of compressive strains in the drawn stress-strain curves [41]. For
capturing the deformation behavior of fabricated OPTS during
compression testing, a Dino lite video camera was utilized with 50 fra­
mes/sec. In order to validate the deformation mechanism of fabricated
OPTS with experimental results, the Gibson-Ashby model [42],
mentioned as equation (3), was used
( )
IOPTS ρOPTS n
=C (3)
Ibulk ρbulk

where, IOPTS denote the calculated mechanical property of fabricated

OPTS and Ibulk represent the bulk property of iron; ρOPTS signify the
measured density of fabricated OPTS, ρbulk where denote the bulk den­
sity of iron; C and n represent the fitting constants. The value of C was
depended upon the size and shapes of the pore of fabricated foam, and
the n value depends on the deformation mechanism governed during
compression.
The energy absorption capacity (Ev ) and energy absorption efficiency
(η) of the fabricated OPTS was determined by the area under the
compressive stress-strain curve using the ISO standard 13,314 [41]. The
energy absorbed per unit volume, and energy absorption efficiency was
defined by equations (4) and (5).
∫εmax
Ev = σdε (4)
0

Fig. 4. Details of CAD design, 3D printed green part and fabricated part of
OPTS with different pore and strut size.

4
D.K. Mishra and P.M. Pandey Materials Science & Engineering A 804 (2021) 140759

∫εmax technique. The cross-section of different unit cells and pore shapes
σdε namely cubic and hexagonal of developed OPTS can be seen in Fig. 5.
The developed OPTS displayed neither partial construction of struts nor
η= 0
(5)
σmax × εmax pore blocking. It may be inferred that better diffusion between the metal
particles was observed which further induced strong bonding even
where σ and ε denote compressive engineering stress and strain, εmax
represents maximum compressive engineering strain, σ max denotes
maximum compressive engineering stress corresponding to maximum
compressive engineering strain.

3. Results

3.1. Morphological characterization

Fig. 4 show the OPTS of iron with different pore shape and strut sizes
fabricated successfully using developed fabrication methodology. It
could be inferred from Fig. 4 that the interconnected pore architecture of Fig. 6. SEM image (at 2KX) of fabricated strut (a) without polished, and (b)
the desired CAD model can be printed successfully using the fabrication polished with 5% nital etched surface.

Fig. 5. Details of different strut and pore sizes with measurements of (a) C-1.0 mm, (b) C-1.25 mm, (c) C-1.5 mm, (d) H-1.0 mm, (e) H-1.25 mm, and (f) H-1.5 mm.

5
D.K. Mishra and P.M. Pandey Materials Science & Engineering A 804 (2021) 140759

without the application of external pressure and the same can be Table 2
observed from the SEM image (refer to Fig. 6 (a)). The presence of mi­ Porosity and relative density details of developed OPTS.
cropores in the fabricated strut of OPTS could be seen from 5% nital Sample Features Designed Measured Variation Relative
etched SEM micrograph (refer to Fig. 6 (b)). The resulted microporosity designs porosity porosity (%) (%) density
on the strut surface was obtained due to the pressureless sintering of 3D (%) (%)
printed green parts [8,43]. Cubic C-1 38 50 ± 1.05 31.58 50
The absence of external pressure during processing may reduce C-1.25 30 39 ± 1.30 30.00 61
bonding between the particles, which also resulted in micro-voids [8]. In C-1.5 28 31 ± 1.20 10.47 69
the present study, microporosity observed in the fabricated parts was a Hexagonal H-1 55 64 ± 1.04 16.36 36
H-1.25 42 55 ± 1.60 30.95 45
result of the sintering process performed at the optimum condition. H-1.5 36 44 ± 1.20 22.22 56
Thus, the fabricated OPTS have macro-pores as per the design of the
CAD model and micro-pores due to the voids between metal particles
(CIPs).
The dimensional study of strut size (i.e. cell wall thickness) and pore
size of fabricated OPTS was performed by Dino-Lite optical camera
which can be seen in Fig. 5. The dimensional variation of fabricated
OPTS from the designed CAD model is shown in Table 1. It is apparent
that the dimensions of fabricated pore size vary from 0.6 to 3.3 %, and
cell wall thickness varies from 1 to 6 % from the intent CAD model. The
details of porosity and relative density of fabricated OPTS are presented
in Table 2. The porosity obtained using the developed fabrication
technique was found between the ranges of 31 to 64 %. Moreover, it
could be inferred from Table 2 that the measured porosity (%) of
fabricated samples were obtained higher as compared with designed
porosity (%). The variations in the porosity of samples were measured as
per the technique discussed by Sharma and Pandey [8].

3.2. Mechanical characterization of fabricated OPTS

In the mechanical characterization of fabricated OPTS, the results of

compression tests of developed samples are discussed. The compressive
stress-strain plots of C-OPTS and H-OPTS are shown in Fig. 7. The stress-
strain plots are represented in a set of three curves and each curve has
been divided on the cell wall thickness like1.0 mm, 1.25 mm, and
1.5 mm, respectively. The stress-strain curves were categorized into
three different regions such as (i) elastic region, (ii) plateau region, and
(iii) densification region. In an elastic region, stresses were increased
linearly with deformations due to cell wall bending, thus the region
showed an elastic behavior. Second, in the plateau region stresses were
observed to vary with the little amount due to the collapsing of the cell
wall. In the densification portion of the stress-strain curve, stresses were
found to increase abruptly due to the complete collapsing of the cell. As
a result, a further increase in strain compresses the body itself.
Fig. 7 (a) shows the compressive stress-strain plot of C-1, C-1.25, and
C-1.5, respectively. It could be observed that the oscillating value of
stress was found in the plateau region. This would be the failure of the
brittle cell wall [42]. Additionally, the C-OPTS samples exhibited a Fig. 7. Compressive stress-strain plot of fabricated (a) C-OPTS, and (b)
shorter plateau region as compared to H-OPTS. The compressive H-OPTS.
stress-strain plots of H-1, H-1.25, and H-1.5 can be inferred from Fig. 7
(b). The deformation behavior of H-OPTS samples was found similar to compression, namely compressive Young’s modulus (Ec ), ultimate
the nature of elastic-plastic foam [42]. It is also be observed by exam­ compressive stress(UCS), plateau stress (σ pl ), and compressive yield
ining the stress-strain plot of H-OPTS that the plateau region obtained strength (σy ) were calculated according to ISO standard 13314 [41]. The
was smoother and longer as compared to C-OPTS samples. effects of dissimilar strut sizes of fabricated OPTS on different me­
In the present study, four different mechanical properties in chanical properties were discussed and presented in Figs. 8 and 9,

Table 1
Dimensional variations of fabricated OPTS.
Sample design Features Designed dimensions (mm) Pore size Strut size

Pore size Strut size Measured (mm) Deviation (%) Measured (mm) Deviation (%)

Cubic C-1 2.0 1.0 2.04 ± 0.02 2 0.99 ± 0.13 1

C-1.25 1.75 1.25 1.74 ± 0.03 0.6 1.20 ± 0.02 4
C-1.5 1.5 1.5 1.45 ± 0.02 3.3 1.41 ± 0.01 6
Hexagonal H-1 2.0 1.0 1.96 ± 0.04 2 1.04 ± 0.03 4
H-1.25 1.75 1.25 1.72 ± 0.01 1.7 1.24 ± 0.02 1
H-1.5 1.5 1.5 1.55 ± 0.005 3.3 1.41 ± 0.04 6

6
D.K. Mishra and P.M. Pandey Materials Science & Engineering A 804 (2021) 140759

Fig. 8. Effect of variation of cell wall thickness on (a) compressive Young’s

modulus, and (b) ultimate compressive strength. Fig. 9. Effect of variation of cell wall thickness on (a) Plateau stress, and (b)
compressive yield strength.
respectively. The C-OPTS was found to have higher mechanical prop­
erties as compared to H-OPTS. It could be credited to the presence of variations obtained in fabricated scaffold using the developed method­
lower porosity in the cell wall thickness of fabricated C-OPTS. A similar ology were found comparatively less as compared to the techniques [8,
finding was also discussed in the available literature [43]. Moreover, the 43,45]. After comparing it with the designed CAD model, it could be
energy absorption capacity and energy absorption efficiency of fabri­ inferred that the cell wall thickness was observed to decrease, and the
cated foams were also evaluated using equations (4) and (5), respec­ pore size was found to increase. The dimensional variation in the
tively. The energy absorption capacity of developed foams was found to fabricated cell wall and pore size could be credited to the movement and
the maximum compressive strain obtained during compression testing misorientation of spherical CIPs during pressureless microwave sinter­
[44]. It could be inferred from Fig. 10 that the energy absorption ca­ ing [8,36,43] In the first instance, the CIPs were loosely bonded with the
pacity of fabricated C-OPTS has a higher value as compared to H-OPTS. polymer (binder) in the 3D printed parts as no external pressure was
In context to cell wall thickness, the higher cell wall thickness possesses applied before sintering as observed from Fig. 13 (a). When the first
higher energy absorption capacity to lower cell wall thickness of stage of thermal debinding was completed during microwave sintering,
developed OPTS (refer to Fig. 11). Moreover, the effect of different cell an ample amount of pores between the metal particles were generated
wall thickness on the energy absorption efficiency of fabricated OPTS (can be inferred from Fig. 13 (b)). These pores between the metal par­
can be observed in Fig. 12. From the stress-strain diagram (refer to ticles acted as a free space for surrounding or adjacent particles. The
Fig. 7), it can be observed that the energy absorbed by the fabricated available free space was covered by the movement of adjacent metal
foam in the elastic stage was found to be less as compared to the plastic particles with a further increase in sintering temperature [38]. These
stage. It could be due to the deformation of pores and cell wall of movements resulted into a necking phenomenon between the CIPs. The
fabricated OPTS during plastic stage of deformation [44]. Moreover, it necking phenomenon resulted in the formation of the concave surface
was found in a prior study [44], that lesser porosity and smaller pore size within the CIPs. Therefore, the attraction between the convex surface of
of fabricated foam was responsible for absorbing higher energy. spherical CIPs and the concave surface formed at the neck resulted in the
misorientation of CIPs [8]. Additionally, it was reported in the prior
4. Discussion study [46] that the microwave sintering of CIPs induced high grain
boundary surface diffusion during the sintering temperature range of
4.1. Morphological study (800 − 900◦ C). Therefore, the effect of high grain boundary surface
diffusion led to an increase in the fraction of grain boundaries misori­
From Table 1, it could be inferred that the variation in dimensions of entation angle within the CIPs [46]. Consequently, more inter-particle
the cell wall thickness and pore size was found to vary from 1 to 6% and shrinkage was observed during pressure-less microwave sintering
0.6 to 3.3% with respect to the designed CAD model. However, which further resulted in dimensional variation [46]. Besides, reducing

7
D.K. Mishra and P.M. Pandey Materials Science & Engineering A 804 (2021) 140759

Fig. 10. Energy absorption capacity of (a) C-OPTS, and (b) H-OPTS.
Fig. 12. Effect of cell wall thickness on energy absorption efficiency of fabri­
cated (a) C-OPTS and (b) H-OPTS.

reasons could be variations in dimensions of strut and pore size were

attributed to inter-particle shrinkage due to pressureless microwave
sintering and post-processing cleaning due to sandblasting. The varia­
tion in porosity because of pressureless microwave sintering on the
different cell wall thicknesses can be seen from 5% nital etched optical
micrograph (refer to Figs. 14 and 15). It was evident from Figs. 14 and
15 that porosity contents in the hexagonal based OPTS were obtained
higher as compared to cubic based OPTS. This porosity represents the
inherent microporosity in the fabricated cell wall. The obtained range of
porosity variations in the present study was found quite low
(10 to ​ 32 %) as compared to the prior study performed by Sharma and
Pandey [8]. Therefore, it could be reduced further by selecting proper
metallic ink composition [47] with suitable sintering parameters.
Furthermore, the post-processing cleaning had also played a major role
in increased variation in dimensional characteristics. During sand
blasting, spherical shape metal particles became flat as when
high-pressure flow of glass bead impacted on the surface. As a result, the
surface roughness of the sintered cell wall of fabricated OPTS was
Fig. 11. Effect of different cell wall thickness on energy absorption capacity of
reduced after sand-blasting [43]. The variation in dimensional charac­
fabricated OPTS. teristics could be controlled in an effective way by utilizing fine sized
glass bead in sand-blasting or using another way to improve surface
finishing such as electropolishing [8]. From Table 2, it can be observed
materials due to the post-processing step such as sandblasting or surface
that the developed methodology will be capable of fabricating the iron
cleaning was also found responsible for dimensional variations.
foam with different values of densities. Therefore, the overall changes in
Furthermore, using the developed fabrication technique, the devia­
the cell wall thickness and pore size of different manufactured foam was
tion in porosity of fabricated samples was found to vary between the
credited to a change in relative density. Apart from the morphological
ranges of 10 to ​ 32 % (refer to Table 2). These variations in porosity
study, it is apparent that using the developed technique, the
were obtained due to changes in dimensions of strut and pore size. The

8
D.K. Mishra and P.M. Pandey Materials Science & Engineering A 804 (2021) 140759

Fig. 13. Image captured of printed sample using SEM (a) before, and (b) after
thermal debinding.

macroporosity, and microporosity in the form of different cell wall

thicknesses and a unit cell can be fabricated. Moreover, the level of
macorporosity could be tuned using a user defined in CAD design.
Hence, the developed technique can fabricate any complex structure,
especially sandwich structure or graded engineered material structure.

4.2. Mechanical characterization

Fig. 14. Optical microscopic images of C-OPTS having cell wall thickness of (a)
C-1.0 mm, (b) C-1.25 mm, and (c) C-1.5 mm.
4.2.1. Study of compressive behavior of produced foams
The wide range of Young’s modulus and other mechanical properties
C-OPTS and H-OPTS was found different in the current work. Initially,
decreased with increased porosity in fabricated foams. Due to its tunable
the stress increased linearly with strain until deformation occurred in
mechanical properties, the developed foams enabled them to find their
C-OPTS by yielding, bending, and buckling of cell walls (i.e., struts). It
uses in various technical fields, especially in the biomedical area. For
can be deduced from Fig. 16 (a) that at 20% strain the microplastic
biomedical application, the wide range of Young’s modulus, compatible
deformation occurred by the formation of local stress raisers at bonding
with the human bone matrix are essential to reduce the chance of stress
necks due to the presence of cell wall microporosity (refer to Fig. 14 (a)).
shielding.
Here, these cell wall microporosity acts as a prone site for stress con­
In the present section, the compressive behavior of fabricated C-
centration during the action of compressive loading. In a prior study
OPTS and H-OPTS were captured using a Dino-lite camera which can be
[48], it was reported that the effect of microporosity resulted in the
inferred from Figs. 16 and 17. Moreover, it was reported [48] that the
reduction of compressive strength.
deformation behavior of an ordered pore structure was mainly depen­
After reaching the stage of macroscopic plastic deformation, the cell
dent upon the cell topology. Similarly, the compressive behavior of

9
D.K. Mishra and P.M. Pandey Materials Science & Engineering A 804 (2021) 140759

the deformations of cell walls during action of compressive loading

induced sharp variations of stress in plateau region. The sharp variation
of plateau stress could be the clear evidence of brittle failure of cell wall
(region enclosed in yellow circle in Fig. 16) [8]. These brittle failures of
cell wall behavior were found more predominant in 1 mm cell wall
thickness of C-OPTS as compared to C-OPTS having 1.25 mm and 1.5
mm cell wall thickness. It could be credited to reduction in relative
density. In addition, the formation of plastic hinges (enclosed in yellow
circle in Fig. 16) and bending of cell wall (enclosed in yellow circle in
Fig. 16) were found responsible for failure of cell walls. Moreover, the
decrease in porosity content from lower to higher cell wall thickness in
C-OPTS (as evident from Fig. 14 (a)) could also found another valid
reason for cell wall to suffer more plastic deformation before failure.
These findings were found similar with the studies reported by other
researchers [8,48]. Besides, it was observed from Figs. 16 and 17 that
the failure of the cell wall started at the center instead of edges in
fabricated OPTS. It could be due to the deposition of more materials at
the edges with respect to the center portion, the center of the cell wall
became a prone site for crack initiation and propagation. The same
reason for crack initiation and propagation was also observed in other
fabricated H-OPTS.
It was noticed that after attaining the small elastic region in H-OPTS
as compared to C-OPTS, the fabricated cell wall started yielding and
bending at 10% strain as shown in Fig. 17 (a). The phenomenon of local
deformation when reached to the next layer of the fabricated cell wall,
the stress again started increasing. Consequently, similar behavior of
yielding, bending, and buckling of cell wall was observed. Moreover,
there existed a formation of shear band approximately at 45◦ during
compressive loading of H-OPTS. From Fig. 17 (c), it can be seen that due
to the formation of shear bands the layers failed diagonally [49]. It could
be because of bending during compressive deformation. Moreover, it
could be seen from Fig. 7 (b) that hexagonal-based OPTS exhibited a
longer plateau region as compared to C-OPTS. Previous study [50]
showed that the length of the plateau region in the stress-strain curve
was mainly related to the total volume content of porosity in the fabri­
cated structure. At low content of porosity (refer to Fig. 14), the plastic
deformation of cell walls occurred at a very lower amount of strain. The
deformation at a lower value of strain resulted in a shorter plateau re­
gion (refer to Fig. 7 (a)). On the contrast, the plastic deformability of cell
walls decreased as porosity content was increased. The decline in plastic
deformability could be connected with the aspect ratio (width/length)
of the cell walls [50]. Since the higher content of porosity (refer to
Fig. 15) lowers the aspect ratio of the cell wall and increases the prob­
ability of the cell wall to deform by buckling. The buckling deformation
resulted into premature failure of cell walls. Therefore, a longer plateau
region can be observed from the compressive stress-strain curve of
H-OPTS (refer to Fig. 7 (a)). Additionally, as deformation continues, the
failed cell walls resulted in an increase in net cross-sectional area and
cause densification of foam.
In order to validate the deformation behavior of fabricated scaffolds,
the Gibson-Ashby model [42] was used to fit with the calculated values
of mechanical properties. The variation in calculated compressive me­
chanical properties such as Young’s modulus, plateau stress, and ulti­
mate compressive stress with respect to relative density is demonstrated
in Fig. 18. As per the Gibson-Ashby model’s equation (3), the value of C
Fig. 15. Optical microscopic images of H-OPTS having cell wall thickness of (a) and n for porous parts are considered as 0.3 and 1.5 respectively [42].
H-1.0 mm, (b) H-1.25 mm, and (c) H-1.5 mm. Therefore, the value of C and n of fabricated porous parts were calcu­
lated using the plots as shown in Fig. 18 and arranged in Table 3. It is
walls started collapsing and then crushing from the weaker and thinner interesting to report here that the determined values of the coefficient of
portions. Consequently, the deformation of cell walls was continued determination (R2) were obtained in the range of 99.5 − 99.9%. More­
until the local deformation reached another row of struts. As local over, it has been reported in the prior studies [51,52], the value of
deformation reached another row of struts, again stress started constant n could be utilized to predict the deformation mechanism of
increasing, and similar deformation such as, yielding, failure and fabricated scaffolds during compressive testing. Yamada et al. [53], re­
crushing of struts were obtained (refer to Fig. 16). Due to the failure of ported that the value of n = 1.0 was allotted for cell wall yielding, n =
cell walls, the deformation bands in fabricated foam was observed along 1.0 to 1.5 for cell wall bending, and n = 2 for cell wall buckling during
the perpendicular direction of the applied compressive load. Moreover, deformation of porous parts in compressive loading. It can be inferred

10
D.K. Mishra and P.M. Pandey Materials Science & Engineering A 804 (2021) 140759

Fig. 16. Mechanical behavior of (a) C-1.0 mm, (b) C-1.25 mm, and (c) C-1.50 mm cell wall thickness under compressive load.

from Table 3 that the value of nE, np and nUCS for C-OPTS was obtained 4.2.2. Effect of cell wall thickness on the mechanical properties of
as1.95, 2.04, and1.89. The obtained value of n for C-OPTS predicted that fabricated parts
failure of cell wall structures occurred due to cell wall yielding, buckling It was noticed from the stress-strain plot (refer to Fig. 7) that as the
and bending. Similarly, for H-OPTS the calculated value of nE, np and thickness of the cell wall increased, the mechanical properties (such
nUCS was estimated as 1.25, 1.69, and 2.5. Hence, it could be observed as Ec UCSσ pl ,σ y ) of fabricated parts were found to increase. The reason
that the failure mechanism of fabricated scaffolds was based on the for an increase in mechanical properties is credited to a decrease in
combination of cell wall yielding, bending and buckling. porosity content of fabricated OPTS. Consequently, the compressive
mechanical properties of C-OPTS were found higher as compared to H-

11
D.K. Mishra and P.M. Pandey Materials Science & Engineering A 804 (2021) 140759

Fig. 17. Compressive behavior of (a) H-1.0 mm, (b) H-1.25 mm, and (c) H-1.50 mm cell wall thickness under compressive load.

OPTS. Moreover, the content of porosity % (can be seen from Figs. 14 increased. Thus, the failure of cell walls occurred due to brittle fracture.
and 15), in the fabricated scaffolds was also found to be a major factor Hence, reduction in porosity resulted into less variation in plateau re­
that affected the energy absorption capacity(Ev )[43]. Therefore, the gion of fabricated OPTS which can be evident from Fig. 7. The following
fabricated C-OPTS possessed a higher energy absorption capacity as result was found similar to the study reported by Aşik and Bor [50].
compared to H-OPTS. On the contrary, the energy absorption efficiency
(η) of fabricated OPTS was found to increase with the increasing porosity 4.2.3. Effect of unit cell shape on the mechanical properties of fabricated
(refer to Figs. 14 and 15) [44]. Moreover, the flat regime of plateau parts
stress in the developed parts indicated the absence of work hardening In the present section, the mechanical properties of two types of unit
[54]. The lack of strengthening mechanisms such as work hardening cells were evaluated during compressive loading. It could be seen from
during compressive loading resulted in lower mechanical strength. Figs. 8 and 9, that mechanical properties of fabricated OPTS were found
Therefore, lesser mechanical strength was obtained in fabricated to significantly different for different unit cells. Among these fabricated
H-OPTS. The fabricated OPTS with have 1 mm cell wall thickness had unit cell-based OPTS, the C-OPTS has exhibited higher mechanical
more variation of stresses in the plateau region as compared to OPTS properties as compared to H-OPTS (refer to Figs. 8 and 9). The reason
with 1.25 mm and 1.5 mm wall thickness because it contained more could be the smaller numbers of stress concentration sites, and sharp
amount of microporosity (can be evident from Figs. 14 and 15), which edges as well as lesser content of porosity (can be seen from Figs. 14 and
acted as a prone site for stress concentration as the compressive load 15), in fabricated C-OPTS [36]. A prior study [8] has been reported that

12
D.K. Mishra and P.M. Pandey Materials Science & Engineering A 804 (2021) 140759

the deformation behavior in the regularly arranged unit cell developed

structures originated from the region close to joints having the
high-stress concentration and sharp edges. Therefore, the stresses were
distributed uniformly in cubic based unit cell OPTS that further resulted
into higher compressive properties (such as Young modulus, yield
strength, and ultimate compressive strength, etc.) [43]. Hence, the
change in porosity due to different type of unit cell shape with the same
wall thickness resulted in altered mechanical properties [8].

4.2.4. Fractured surface analysis

In order to reveal the nature of the fracture, the fractured surface
analysis was performed on failed parts. The fractured SEM images of
fabricated C-OPTS and H-OPTS are shown in Fig. 19. From these SEM
images, it can be deduced that the different microporosity (can be
evident from Figs. 14 and 15) in fabricated scaffolds was obtained.
Therefore, it could be concluded that these variations of microporosity
were found to be a critical factor for the failure of the fabricated sample
during compressive loading. Moreover, a red arrow in the SEM image
(refer to Fig. 19) of the fractured surface shows the sign of plastic
deformation in the sample. The reason could be credited to the perma­
nent distortion of the cell wall during bending [8]. The compressive
loading of the fabricated cell wall resulted in large plastic deformation
before failure which can be observed from Fig. 7. The reason for this
large plastic deformation could be attributed to the failure of the indi­
vidual bonded neck in a ductile manner. In pertinent to mention this, the
portion encircled in red color in Fig. 19 shows ductile dimples between
the fracture joints of metal particles.

5. Comparative study

In order to compare the results of the present study with the prior
work, a brief literature review has been carried out. The results of the
comparative analysis are tabulated in Table 4. It was evident from
Table 4 that the properties obtained from materials prepared using
developed methodology are relatively compatible with human bone
matrix and are analogous to or even better than the reported works.
From the mentioned Table 4, it is pertinent to mention here that fewer
studies have been reported concerning the work related to the fabrica­
tion of regular order porous structure for biodegradable implant
applications.

Fig. 18. Effect of change of relative density on (a) relative compressive Young’s
modulus (b) plateau stress and (c) ultimate compressive strength, respectively.

Table 3
Details of constant values calculated using Gibson-Ashby model.
Unit cell structures Compressive Plateau stress Ultimate
Young’s modulus (MPa) compressive stress
(MPa) (MPa)

CE nE Cp np CUCS nUCS

Cubic 2.57 1.95 2.23 2.04 1.45 1.86 Fig. 19. SEM images (at 2kX) of the failure surfaces of OPTS in compressive
Hexagonal 1.77 1.25 2.0 1.69 1.34 2.5 testing of (a) C-1.0 mm and, (b) H-1.0 mm cell wall thickness.

13
D.K. Mishra and P.M. Pandey Materials Science & Engineering A 804 (2021) 140759

Table 4
Comparative analysis of mechanical and morphological properties of fabricated porous iron.
Material Method of fabrication Porosity (%) Pore morphology Ec (MPa) σpl (MPa) UCS (MPa) References

Cancellous Bone .. 30–95 Irregular 100–5000 .. 2–12 [2,50]

Porous Fe Micro-extrusion based 3D printing + pressure less 3D printing 31–64 Regular 130–257 11–54 11–67 Present study
Porous Fe Indirect solid free form methodology 45.6–87 Regular 200–850 4–21.5 13–52 [8]
Porous Fe Powder metallurgy based space holder technique 32–82 Irregular 0.14–2.59 1.7–71 …. [6]
Porous Mg Selective laser melting 64 Regular 700–800 23–24 …. [51]
Porous Mg Fiber deposition hot pressing 33–54 Regular 100–370 11.1–30.3 … [52]

In the present work, the obtained morphological and mechanical content of porosity in fabricated C-OPTS as compared to H-OPTS
properties of developed porous scaffolds were found comparable to the resulted in a short and fluctuated plateau region.
human cancellous bone and desirable for other biomedical applications. • The compressive mechanical properties such as Young’s modulus,
Moreover, the mechanical strength of the fabricated OPTS was observed plateau stress, yield strength, and ultimate compressive strength of
to be better than the iron scaffolds with random pore distribution. fabricated OPTS were obtained in the range of 136to 257 MPa,
Quadbeck et al. [20], reported that fabricated porous iron showed 11to 54 MPa, 12to 64 MPa, and 11to 67.3 MPa respectively. More­
higher Young’s modulus of elasticity (Ec ) as compared to material over, C-OPTS covered larger stress-strain areas during compressive
developed in current work. It is worth mentioning here that the large deformation that resulted in higher energy absorption capacity than
variation of porosity was achieved in the present materials with respect H-OPTS. Therefore, it can be adduced that C-OPTS possessed higher
to technique discussed in the literatures. The work reported by Capek compressive mechanical strength than H-OPTS.
et al. [6] showed the fabrication of porous iron using powder
metallurgy-based space holder technique. Consequently, a random pore CRediT authorship contribution statement
distribution structure was attained in their study. As we earlier discussed
the random pore distributions resulted in poor mechanical strength in Dipesh Kumar Mishra: Conceptualization, Methodology, Data
the fabricated parts and induced property that made them unsuitable for curation, Writing – original draft, preparation, Visualization, Investi­
biomedical applications. However, Sharma and Pandey [8] showed gation, Formal analysis. Pulak Mohan Pandey: Supervision, Writing -
another study of ordered pore iron based on indirect solid free-form Reviewing & Editing, Project administration, Funding acquisition.
methodology. From Table 4, it is apparent that improved mechanical
properties with comparable porosity of iron were found in the current
study as compared to the study reported by other researchers [8]. Hence, Declaration of competing interest
the present methodology’s obtained results have revealed that the wide
range of mechanical and morphological properties made a good agree­ The authors declare that they have no known competing financial
ment with properties desirable with the human bone matrix. Moreover, interests or personal relationships that could have appeared to influence
micro-extrusion-based 3D printing and pressureless microwave sintering the work reported in this paper.
in the present work resulted in a reduction of fabrication steps compared
to the technique discussed in the available literature. Acknowledgements

6. Conclusions This work was supported by Science and Engineering Research

Board, Department of Science and Technology, New Delhi, India (Grant
The order pore topology structures (OPTS) of pure iron have fabri­ reference no. EMR/2017/001550).
cated successfully using the developed technique based on micro-
extrusion-based 3D printing and pressureless microwave sintering. The References
efficacy of the fabricated unit cell-based OPTS has also been validated
[1] M. Hrubovčáková, M. Kupková, M. Džupon, Fe and Fe-P foam for biodegradable
with the available literature. In the present work, the effect of
bone replacement material: morphology, corrosion behaviour, and mechanical
morphological characteristics on the mechanical behavior of fabricated properties, Ann. Mater. Sci. Eng. (2016) 1–9, https://doi.org/10.1155/2016/
OPTS was reported. The list of concluding points is shown below. 6257368, 00.
[2] S. Wu, X. Liu, K.W.K. Yeung, C. Liu, X. Yang, Biomimetic porous scaffolds for bone
tissue engineering, Mater. Sci. Eng. R Rep. 80 (2014) 1–36, https://doi.org/
• Using the developed methodology, the Cubic and Hexagonal based 10.1016/j.mser.2014.04.001.
unit cell OPTS were fabricated successfully. No evidence of pore [3] H.D. Kim, S. Amirthalingam, S.L. Kim, S.S. Lee, J. Rangasamy, N.S. Hwang,
blockage and an unfabricated cell wall was found in the manufac­ Biomimetic materials and fabrication approaches for bone tissue engineering, Adv.
Healthc. Mater. 6 (2017) 1–18, https://doi.org/10.1002/adhm.201700612.
tured scaffold. Moreover, a wide range of porosity was obtained in [4] L.Z. Fuping Li, Jinshan Li, Tingting Huang, Hongchao Kou*, Compression fatigue
the fabricated scaffolds within the range of 31 to 64 %. In addition, behavior and failure mechanism of porous titanium for biomedical applications.
two different types of porosities, namely macroporosity as per the https://doi.org/10.1016/j.jmbbm.2016.09.035, 2017, 65, 814-823.
[5] M.F. Ashby, T. Evans, N.A. Fleck, J.W. Hutchinson, H.N.G. Wadley, L.J. Gibson,
designed CAD model, and microporosity obtained between bonding Metal Foams: a Design Guide, Elsevier, 2000.
necks of CIPs were found in the fabricated OPTS. [6] J. Čapek, D. Vojtěch, A. Oborná, Microstructural and mechanical properties of
• The dimensional variation in the fabricated cell wall of OPTS was biodegradable iron foam prepared by powder metallurgy, Mater. Des. 83 (2015)
468–482, https://doi.org/10.1016/j.matdes.2015.06.022.
obtained owing to the pressureless sintering of loose CIPs followed [7] F.W.Y.F. Zheng, X.N. Gu, Biodegradable metals, Mater. Sci. Eng. 77 (2014) 1–34.
by post-processing of the fabricated OPTS samples. These dimen­ [8] P. Sharma, P.M. Pandey, Morphological and mechanical characterization of
sional variations were found in the range of 0.6 to 6 % as compared topologically ordered open cell porous iron foam fabricated using 3D printing and
pressureless microwave sintering, Mater. Des. 160 (2018) 442–454, https://doi.
to the designed CAD model.
org/10.1016/j.matdes.2018.09.029.
• It was observed that the porosity content in fabricated iron foam [9] A.H. Yusop, A.A. Bakir, N.A. Shaharom, M.R. Abdul Kadir, H. Hermawan, Porous
significantly affected the micro elastic and macro plastic deformation biodegradable metals for hard tissue scaffolds: A review, Int. J. Biomater. 2012
(2012) 1–10, https://doi.org/10.1155/2012/641430.
during compressive loading. The yielding and bending of cell walls
[10] A. Kumar, P.M. Pandey, Statistical modelling of mechanical properties and bio-
were noticed as the leading cause of failure. Moreover, the small corrosion behaviour of Mg3Zn1Ca15Nb fabricated using microwave sintering,
J. Alloys Compd. 854 (2021) 156211, https://doi.org/10.1016/j.
jallcom.2020.156211.

14
D.K. Mishra and P.M. Pandey Materials Science & Engineering A 804 (2021) 140759

[11] A. Kumar, P.M. Pandey, Study of the influence of microwave sintering parameters [33] S.L. Taylor, A.E. Jakus, R.N. Shah, D.C. Dunand, Iron and nickel cellular structures
on the mechanical behaviour of magnesium-based metal matrix composite, Proc. by sintering of 3D-printed oxide or metallic particle inks, Adv. Eng. Mater. 19
Inst. Mech. Eng. Part C J. Mech. Eng. Sci. (2020), https://doi.org/10.1177/ (2017) 1600365, https://doi.org/10.1002/adem.201600365.
0954406220951236. [34] M. Oghbaei, O. Mirzaee, Microwave versus conventional sintering: A review of
[12] D.K. Pathak, P.M. Pandey, An experimental investigation of the fabrication of fundamentals, advantages and applications, J. Alloys Compd. 494 (2010) 175–189,
biodegradable zinc–hydroxyapatite composite material using microwave sintering, https://doi.org/10.1016/j.jallcom.2010.01.068.
Proc. Inst. Mech. Eng. Part C J. Mech. Eng. Sci. 234 (2020) 2863–2880, https://doi. [35] N.E. Putra, M.A. Leeflang, M. Minneboo, P. Taheri, L.E. Fratila-Apachitei, J.M.
org/10.1177/0954406220910445. C. Mol, J. Zhou, A.A. Zadpoor, Extrusion-based 3D printed biodegradable porous
[13] B. Wegener, B. Sievers, S. Utzschneider, P. Müller, V. Jansson, S. Rößler, B. Nies, iron, Acta Biomater. (2020), https://doi.org/10.1016/j.actbio.2020.11.022.
G. Stephani, B. Kieback, P. Quadbeck, Microstructure, cytotoxicity and corrosion of [36] D.K. Mishra, P.M. Pandey, Mechanical behaviour of 3D printed ordered pore
powder-metallurgical iron alloys for biodegradable bone replacement materials, topological iron scaffold, Mater. Sci. Eng. A (2020) 1–8, https://doi.org/10.1016/j.
Mater. Sci. Eng. B Solid-State Mater. Adv. Technol. 176 (2011) 1789–1796, msea.2020.139293.
https://doi.org/10.1016/j.mseb.2011.04.017. [37] D.K. Mishra, P.M. Pandey, Experimental investigation into the fabrication of green
[14] H. Hermawan, A. Purnama, D. Dube, J. Couet, D. Mantovani, Fe-Mn alloys for body developed by micro-extrusion based 3D printing process, Polym. Compos.
metallic biodegradable stents: degradation and cell viability studies, Acta (2020) 1–17, https://doi.org/10.1002/pc.25514.
Biomater. 6 (2010) 1852–1860, https://doi.org/10.1016/j.actbio.2009.11.025. [38] D.K. Mishra, P.M. Pandey, Effect of sintering parameters on the microstructure and
[15] M. Schinhammer, A.C. Hänzi, J.F. Löffler, P.J. Uggowitzer, Design strategy for compressive mechanical response of porous Fe scaffold fabricated by 3D printing
biodegradable Fe-based alloys for medical applications, Acta Biomater. 6 (2010) and pressure less microwave sintering, Proc. Inst. Mech. Eng. Part C J. Mech. Eng.
1705–1713, https://doi.org/10.1016/j.actbio.2009.07.039. Sci. (2020) 1–16, https://doi.org/10.1177/0954406220921416.journals.sagepub.
[16] D.W. Hutmacher, Scaffolds in tissue engineering bone and cartilage, Biomater. com/home/pic.
Silver Jubil. Compend. 21 (2000) 175–189, https://doi.org/10.1016/B978- [39] O. Cansizoglu, O. Harrysson, D. Cormier, H. West, T. Mahale, Properties of Ti-6Al-
008045154-1.50021-6. 4V non-stochastic lattice structures fabricated via electron beam melting, Mater.
[17] A. Oriňák, R. Oriňáková, Z.O. Králová, A.M. Turoňová, M. Kupková, Sci. Eng. 492 (2008) 468–474, https://doi.org/10.1016/j.msea.2008.04.002.
M. Hrubovčáková, J. Radoňák, R. Džunda, Sintered metallic foams for [40] ASTM B962-13, Standard Test Methods for Density of Compacted or Sintered
biodegradable bone replacement materials, J. Porous Mater. 21 (2014) 131–140, Powder Metallurgy Products Using Archimedes Principle, 2010, https://doi.org/
https://doi.org/10.1007/s10934-013-9757-4. 10.1520/B0962-17.2.
[18] P. Sharma, P.M. Pandey, Corrosion behaviour of the porous iron scaffold in [41] Iso 13314:2011(E), International Standard Mechanical Testing of Metals – Ductility
simulated body fluid for biodegradable implant application, Mater. Sci. Eng. C 99 Testing – Compression Test for Porous and Cellular Metals, 2011.
(2019) 838–852, https://doi.org/10.1016/j.msec.2019.01.114. [42] L.J. Gibson, M.F. Ashby, Cellular Solids (1997), https://doi.org/10.1557/
[19] J. He, F.L. He, D.W. Li, Y.L. Liu, D.C. Yin, A novel porous Fe/Fe-W alloy scaffold mrs2003.79.
with a double-layer structured skeleton: preparation, in vitro degradability and [43] G. Singh, P.M. Pandey, Uniform and graded copper open cell ordered foams
biocompatibility, Colloids Surf. B Biointerfaces 142 (2016) 325–333, https://doi. fabricated by rapid manufacturing: surface morphology, mechanical properties and
org/10.1016/j.colsurfb.2016.03.002. energy absorption capacity, Mater. Sci. Eng. 761 (2019) 1–14, https://doi.org/
[20] P. Quadbeck, R. Hauser, K. Kümmel, G. Standke, G. Stephani, B. Nies, S. Rößler, 10.1016/j.msea.2019.138035.
B. Wegener, Iron based cellular metals for degradable synthetic bone replace-ment, [44] J. Chen, X. Li, W. Li, C. Li, B. Xie, S. Dai, J.J. He, Y. Ren, Research on energy
Proc. World Powder Metall. Congr. Exhib. World PM 4 (2010) (2010) 1–8. absorption properties of open-cell copper foam for current collector of Li-ions,
[21] A.A. Plunk, D.C. Dunand, Iron foams created by directional freeze casting of iron Mater. Sci. Pol. 37 (2019) 8–15, https://doi.org/10.2478/msp-2019-0011.
oxide, reduction and sintering, Mater. Lett. 191 (2017) 112–115, https://doi.org/ [45] J.P. Singh, P.M. Pandey, A.K. Verma, Fabrication of three dimensional open porous
10.1016/j.matlet.2016.12.104. regular structure of PA-2200 for enhanced strength of scaffold using selective laser
[22] J. Čapek, D. Vojtěch, Microstructural and mechanical characteristics of porous iron sintering, Rapid Prototyp. J. 22 (2016) 752–765, https://doi.org/10.1108/RPJ-11-
prepared by powder metallurgy, Mater. Sci. Eng. C 43 (2014) 494–501, https:// 2014-0148.
doi.org/10.1016/j.msec.2014.06.046. [46] S. Kehrein, Modern Developments, Springer science & Business media, LLC, 1966,
[23] B.T.L. Nguyen, M.P. Staiger, G.J. Dias, T.B.F. Woodfield, A Novel Manufacturing p. 2006.
Route for Fabrication of Topologically - Ordered Porous A Novel Manufacturing [47] N. Paxton, W. Smolan, T. Böck, F. Melchels, J. Groll, T. Jungst, Proposal to assess
Route for Fabrication of Topologically-Ordered Porous Magnesium Scaffolds **, printability of bioinks for extrusion-based bioprinting and evaluation of rheological
2011, https://doi.org/10.1002/adem.201100029. properties governing bioprintability Proposal to assess printability of bioinks for
[24] D.D. Gu, W. Meiners, K. Wissenbach, R. Poprawe, Laser additive manufacturing of extrusion-based bioprinting and evaluation of rheological properti, Biofabrication
metallic components: materials, processes and mechanisms, Int. Mater. Rev. 57 9 (2017) 1–18.
(2012) 133–164, https://doi.org/10.1179/1743280411Y.0000000014. [48] O. Al-Ketan, R. Rowshan, R.K. Abu Al-Rub, Topology-mechanical property
[25] L.E. Murr, S.M. Gaytan, F. Medina, H. Lopez, E. Martinez, B.I. MacHado, D. relationship of 3D printed strut, skeletal, and sheet based periodic metallic cellular
H. Hernandez, L. Martinez, M.I. Lopez, R.B. Wicker, J. Bracke, Next-generation materials, Addit. Manuf. 19 (2018) 167–183, https://doi.org/10.1016/j.
biomedical implants using additive manufacturing of complex cellular and addma.2017.12.006.
functional mesh arrays, Philos. Trans. R. Soc. A Math. Phys. Eng. Sci. 368 (2010) [49] J. Kadkhodapour, H. Montazerian, A.C. Darabi, A. Zargarian, S. Schmauder, The
1999–2032, https://doi.org/10.1098/rsta.2010.0010. relationships between deformation mechanisms and mechanical properties of
[26] S. Bose, S. Vahabzadeh, A. Bandyopadhyay, Bone tissue engineering using 3D additively manufactured porous biomaterials, J. Mech. Behav. Biomed. Mater. 70
printing, Mater. Today 16 (2013) 496–504, https://doi.org/10.1016/j. (2017) 28–42, https://doi.org/10.1016/j.jmbbm.2016.09.018.
mattod.2013.11.017. [50] E.E. Aşik, Ş. Bor, Fatigue behavior of Ti-6Al-4V foams processed by magnesium
[27] P. Heinl, L. Müller, C. Körner, R.F. Singer, F.A. Müller, Cellular Ti-6Al-4V space holder technique, Mater. Sci. Eng. 621 (2015) 157–165, https://doi.org/
structures with interconnected macro porosity for bone implants fabricated by 10.1016/j.msea.2014.10.068.
selective electron beam melting, Acta Biomater. 4 (2008) 1536–1544, https://doi. [51] M. Hakamada, Y. Asao, T. Kuromura, Y. Chen, H. Kusuda, M. Mabuchi, Density
org/10.1016/j.actbio.2008.03.013. dependence of the compressive properties of porous copper over a wide density
[28] B. Gorny, T. Niendorf, J. Lackmann, M. Thoene, T. Troester, H.J. Maier, In situ range, Acta Mater. 55 (2007) 2291–2299, https://doi.org/10.1016/j.
characterization of the deformation and failure behavior of non-stochastic porous actamat.2006.11.024.
structures processed by selective laser melting, Mater. Sci. Eng. 528 (2011) [52] D.P. Mondal, M. Patel, S. Das, A.K. Jha, H. Jain, G. Gupta, S.B. Arya, Titanium foam
7962–7967, https://doi.org/10.1016/j.msea.2011.07.026. with coarser cell size and wide range of porosity using different types of
[29] Y. Li, H. Jahr, K. Lietaert, P. Pavanram, A. Yilmaz, L.I. Fockaert, M.A. Leeflang, evaporative space holders through powder metallurgy route, Mater. Des. 63 (2014)
B. Pouran, Y. Gonzalez-Garcia, H. Weinans, J.M.C. Mol, J. Zhou, A.A. Zadpoor, 89–99, https://doi.org/10.1016/j.matdes.2014.05.054.
Additively manufactured biodegradable porous iron, Acta Biomater. 77 (2018) [53] Y. Yamada, C. Wen, K. Shimojima, H. Hosokawa, Y. Chino, M. Mabuchi,
380–393, https://doi.org/10.1016/j.actbio.2018.07.011. Compressive deformation characteristics of open-cell Mg alloys with controlled cell
[30] P. Sharma, P.M. Pandey, A novel manufacturing route for the fabrication of structure, Mater. Trans. 43 (2002) 1298–1305, https://doi.org/10.2320/
topologically-ordered open-cell porous iron scaffold. https://doi.org/10.1016/j. matertrans.43.1298.
matlet.2018.03.206, 2018, 222, 160-163. [54] V. Sharma, N. Grujovic, F. Zivic, V. Slavkovic, Influence of porosity on the
[31] A. Panwar, L.P. Tan, Current status of bioinks for micro-extrusion-based 3D mechanical behavior during uniaxial compressive testing on Voronoi-based open-
bioprinting, Molecules 21 (2016), https://doi.org/10.3390/molecules21060685. cell aluminium foam, Materials 12 (2019), https://doi.org/10.3390/ma12071041.
[32] M. Vaezi, G. Zhong, H. Kalami, S. Yang, Extrusion-based 3D Printing Technologies
for 3D Scaffold Engineering, Elsevier Ltd, 2017, https://doi.org/10.1016/B978-0-
08-100979-6.00010-0.

15