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The study of mechanical properties of poly(lactic) acid PLA-based 3D printed

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journal homepage: www.elsevier.com/locate/matpr

The study of mechanical properties of poly(lactic) acid PLA-based 3D

printed filament under temperature and environmental conditions
Ahmad Adnan Bin Abu Bakar a, Muhammad Zulhilmi Bin Zainuddin a, Ahmad Nurhelmy Bin Adam a,
Ikhwan Syafiq Bin Mohd Noor b, Nizam Bin Tamchek c, Muhammad Syafiq Bin Alauddin a,d,
Mohd Ifwat Bin Mohd Ghazali a,⇑
a
SMART RG, Faculty Science and Technology, Universiti Sains Islam Malaysia (USIM), 71800 Nilai, Negeri Sembilan, Malaysia
b
Physics Division, Centre of Foundation Studies for Agricultural Science, Universiti Putra Malaysia, 43400, UPM, Serdang, Selangor, Malaysia
c
Department of Physics, Universiti Putra Malaysia, Serdang, Selangor, Malaysia
d
Department of Conservative Dentistry and Prosthodontics, Faculty of Dentistry, Universiti Sains Islam Malaysia, Kuala Lumpur 56100, Malaysia

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

Article history: Recently, Industrial Revolution 4.0 has highlighted the key components that will shift the world into dig-
Available online xxxx italization; cybersecurity, cloud computing, mobile technologies, machine to machine, advanced robotics,
big data, Internet of Things (IoT), RFID technology, cognitive computing and additive manufacturing.
Keywords: Additive manufacturing or better known as 3D printing technology has captivated many researchers
Additive manufacturing (AM) due to its many advantages. This study aims to focus on the influence of temperature on the physical
Poly(lactic acid) (PLA) properties of the 3D printed structure made from poly(lactic) acid (PLA) with 100% infill. The highest
Post-heat treatment
Young’s modulus at the value of 4.42 GPa was obtained with a slight deviation under other samples
Tensile
Sustainability
exposed at the temperature of 70 °C and 80 °C. It was found that the ultimate tensile strength of the
3D printed structure when being exposed at the temperature of 80 °C for a maximized duration of 10 days
while the breakage/fracture limit was recorded on samples after the 13rd day exposure at the same tem-
perature. Meanwhile, the highest strain was achieved at 8.04% also during the 13rd day but at 70 °C. In
conclusion, post-heat treatment has minimal effect on the Young’s modulus of 3D printed PLA but it was
largely effecting the fracture limit of the structure. Therefore, heat treatment at temperature closed to the
glass transition temperature of PLA polymer improved the adhesion strength between the printed layer
thus enhancing the durability of the specimen under load conditions.
Ó 2022 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the International Confer-
ence on ‘‘Recent Advances in Functional Materials”.

1. Introduction chemicals and gasses, the wasteful utilization of raw materials,

Industrial Revolution 4.0 has altered and provided a paradigm
shift in our daily lives by overhauling the industrial sectors to
accommodate automation, the internet of things, and customiza-
tion. The manufacturing industry is one of the most vibrant indus-
tries that help boost the economy; financially and socially [1]. The
industry provides ample opportunities for research, employability,
and innovation. However, manufacturing technology has also been
considered as one of the main reasons for environmental issues.
The technology requires facilities and equipment that impact the
environment in several factors in particularly the emission of
⇑ Corresponding author.
E-mail address: ifwat.ghazali@usim.edu.my (Mohd Ifwat Bin Mohd Ghazali).
and increased disposable waste [2,3].
As an alternative, several manufacturing technologies have
been invented and innovated to address environmental problems.
One of the technologies that have recently revolutionized the man-
ufacturing industry is additive manufacturing technology, popu-
larly known as 3D printing technology. 3D printing technology is
a technology that utilizes computer-aided design (CAD) design
and transforming the design into a 3D object by using layer upon
layer built setup [4]. 3D printing technology can be categorized
in various techniques, which include vat-polymerization, sheet
lamination, directed energy deposition, binder jetting, material jet-
ting, powder bed fusion, and material extrusion [5,6]. The revolu-
tion of 3D printing technology has provided a new outlook on
manufacturing by transforming the process of fabrication to a

https://doi.org/10.1016/j.matpr.2022.06.198
2214-7853/Ó 2022 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the International Conference on ‘‘Recent Advances in Functional Materials.

Please cite this article as: Ahmad Adnan Bin Abu Bakar, Muhammad Zulhilmi Bin Zainuddin, Ahmad Nurhelmy Bin Adam et al., The study of mechanical properties of poly(lactic)
acid PLA-based 3D printed filament under temperature and environmental conditions, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2022.06.198
Ahmad Adnan Bin Abu Bakar, Muhammad Zulhilmi Bin Zainuddin, Ahmad Nurhelmy Bin Adam et al.
cost-effective, energy-friendly usage rate, reduction of raw mate-
rial waste, and environmentally friendly process [7,8].
Among the commonly used techniques of 3D printing is the
material extrusion process familiarly known as the fused deposi-
tion modeling (FDM) process which is widely used due to its
affordability, easy to use, good accuracy, rapid prototyping, and
scalability. The FDM process involves the deposition of material
(3D printed filament) through an extruder with specific
temperature-dependent of material properties to be extruded in
a layer upon layer orientation onto a heated bed based on the
desired design. In recent years the utilization of 3D printing tech-
nology can be seen in a plethora of applications, including in aero-
space, automotive, robotics, construction, dentistry, and the
medical sector. The utilization of 3D printing became more evident
during the pandemic where 3D printing is used as a manufacturing
tool to fabricate medical devices such as personal protective equip-
ment (face shield and respirators), testing devices (Nasopharyngeal
swabs), and medical devices (ventilator parts including valve and
components). This is possible as the materials used are made of
medical-grade properties to ensure the performance is on par with
the application’s needs.
In 3D printing technology, the material is an important feature
in achieving the desired performance, notably for the mechanical
properties by using various methods, including blending, polymer-
ization and metal matrix composites (MMCs). Metal matrix com-
posites (MMCs) is a composite material that typically dispersed
reinforce material within the metal matrix such as steel, alu-
minium or copper [9]. The notion of this materials is to compensate
with the heavy-weight characteristic of metal whilst maintaining
the mechanical properties such as higher strength, higher ductility
and better tribological performance [10]. However, high manufac-
turing costs and limited technical expertise have become con-
straints for the usage of MMCs [11]. Amongst the most
promising 3D printing material is poly(lactic) acid (PLA) which is
derived from renewable resources like corn starch and sugar cane.
PLA emerged as a desirable candidate as it is eco-friendly
(biodegradable), biocompatible (non—toxic), and processable (bet-
ter thermal properties). The properties of PLA provide the polymer
several advantages as compared to a conventional polymer such as
acrylonitriles butadiene styrene (ABS). PLA provides a stiffer attri-
bute than ABS. However, the disadvantage of PLA is the heat-
tolerant capabilities and chemical resistance. As 3D printing tech-
nology evolves, the sustainability aspect is important to maintain
eco-friendly conditions and retaining the performance needed for
a specific application. The ecosystem of 3D printing is usually illus-
trated in Fig. 1 where the printed object can be recycled or placed
in landfills to be degraded.
In order to achieve a good stabilization of product performance
and environmental friendliness, manufacturers must include prin-
Fig. 1. 3D printing eco-system.
2
Materials Today: Proceedings xxx (xxxx) xxx
ciples such as green chemistry, sustainability, and engineering
them into their research and development (R&D). Enhancing
matrix crystallization has shown to be a successful method for pro-
ducing heat-resistant PLA. The heat resistance of the polymer could
be greatly improved by both thermal annealing and nucleating
agent which later will induce the matrix crystallization structure
of the polymer [12]. As we know, the temperature is one of the fac-
tors that will affect the rate of crystallization despite other factors
such as polymer structure, polymer chain, cooling rate and molec-
ular weight. Increase in the crystallinity of polymer will directly
affect its mechanical properties, especially the tensile stress and
strains. However, in many situations, increasing matrix crys-
tallinity alone will not improve toughness since the proper shape
is required for PLA matrix to undergo plastic deformation [13].
Other than that, the use of biopolymer is one of the ways to
maintain sustainability in the environment compared to a conven-
tional polymer as most of the biopolymers derived from living
organisms. They have all existed on our planet for millions of years,
giving microbes ample time to create enzymes capable of destroy-
ing their structure making them biodegradable. In general, their
end life does not have a significant impact on the environment,
but the thing goes different when the degradation of biopolymer
undergoes in-appropriate conditions. A landfill, is one example of
unsuitable condition for this process, as it lacks oxygen and water,
making it incompatible for biodegradation. The biopolymer will
decompose in the absence of oxygen (anaerobic process), releasing
biomass, methane (CH4), carbon dioxide (CO2) and water as well as
other tiny molecules to the environment. As we know, methane is
a far more powerful global warming gas than carbon dioxide
because it is not easily absorbed by plants [14].
In this work, white filament has been chosen among other col-
ors since previous study reported that it has higher tensile
strength [15]. According to a study, the recommended annealing
temperature of the polymer to improve the mechanical properties
must be greater than the glass transition temperature and less
than the melting point [16]. The research focuses on the mechan-
ical properties of the 3D printed specimen expose to different
thermal conditions (23 °C, 32 °C, 70 °C and 80 °C) for a period
of time (31 days = a month). The glass transition of 3D printed
PLA varies from 55 °C until 65 °C. Thus, two temperatures below
glass transition had been chosen simulate the effect of indoor and
outdoor environment; 23 °C and 32 °C respectively, whilst the
latter slightly above the glass transition had chosen to avoid
warping; 70 °C and 80 °C. The thermal effects towards the 3D
printed filaments will be studied in terms of the physical and
mechanical properties of the specimens by using the measured
Young’s modulus to understand the effect of heat and duration.
In addition, the images of 3D printed specimens are studied to
assess the potential changes of the physical adhesion between
printed layers.
2. Experimental procedure
The study will be conducted to understand the effect of various
temperatures (heat treatment) on the 3D printed PLA specimens.
The physical properties will be observed to study the changes in
the structure of the 3D printed PLA specimens. Triplicate of 3D
printed PLA specimens were printed for each test (a total of 123
for overall study) to provide significant statistical relevancy.
2.1. Specimens preparation
White PLA filament (Flashforge, Zhejiang Flashforge 3D Tech-
nology Co. Ltd.) with density of 1.25 g/cm3 and the melting tem-
perature (Tm) of 176 °C was utilized for this research. The
Ahmad Adnan Bin Abu Bakar, Muhammad Zulhilmi Bin Zainuddin, Ahmad Nurhelmy Bin Adam et al. Materials Today: Proceedings xxx (xxxx) xxx

Fig. 2. (a) The dog-bone specimen specifications according to the ASTM D-638; (b) Ender-3 Pro printer used in this research.

structure to be printed was according to ASTM D-638. The dimen-
sion of the structure is illustrated in Fig. 2(a). Prior to 3D printing,
the structure of the design was done using a CAD software,
Fusion360. The design was then converted using slicer (Ultimaker
Cura 4.7) as a g-code file and sent to 3D printer (Ender-3 Pro) as
indicated in Fig. 2(b) with 100% infill specification. A total of 123
3D printed PLA specimens were fabricated. Before exposing to
the thermal conditions, the 3D printed PLA specimens were
weighted for the initial condition using an electronic weight
machine and the data were recorded.
2.2. Temperature conditions
To study the effect of temperature on the 3D printed PLA spec-
imens, the specimens had been exposed to four thermal conditions
(23 °C, 32 °C, 70 °C and 80 °C) as illustrated in Fig. 3. The 3D printed
PLA specimens had been subjected to the conditions for certain
days within a month. After a period of time, the 3D printed PLA
specimens were weighed once again as a final weight data and
underwent the tensile measurement using Universal Testing
Machine (UTM).
2.3. Measurement of tensile properties of the PLA based on 3D printed
structure
Preparatory to the tensile test, the 3D printed PLA specimens
were left to cool down for about an hour to ensure the tensile test-
ing must be done when the specimens reached at 23 °C (room tem-
perature). The stress–strain measurement was conducted
according to ASTM D-638, using Instron 5565 Universal Testing
Machine (UTM) fitted with a 30 kN load cell and operated at a
cross-head speed of 50 mm/min. The parameters of the printing
approach are shown in Table 1. The load direction relative to the
layer direction in printing the specimen was 45° as shown in
Fig. 4. Bluehill software was used to record the tensile data such
as tensile stress, tensile strain and Young’s modulus.
3. Results and discussion
3.1. Influence of temperature conditions on tensile properties towards
3D printed PLA with 100% infill
Triplicate specimens were tested for each stress–strain curve
and the mean values are presented as a result. Fig. 5(a) shows

Fig. 3. Four temperature conditions for 3D printed PLA specimens heat treatment.

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Ahmad Adnan Bin Abu Bakar, Muhammad Zulhilmi Bin Zainuddin, Ahmad Nurhelmy Bin Adam et al. Materials Today: Proceedings xxx (xxxx) xxx

Table 1 day. But only on the 24th day and day 31st were recorded at
The parameter settings approach of 3D printed PLA specimens. 4.94% and 3.97% respectively. As expected, the increasing temper-
Parameters Values ature of heat treatment produces a significantly higher strain at
Layer Height (mm) 0.2 failure. The material is considered brittle when it fractures with lit-
Wall Line Count 2 tle elastic deformation and without significant plastic deformation
Wall Thickness (mm) 0.8 (tensile strain). As the PLA is a semi-crystalline polymer, its amor-
Infill Density (%) 100 phous region enables the free carbon chain to experience the tran-
Infill Pattern Lines
Print Speed (mm/s) 50
sition from the rigid to rubbery-like phase [17]. The free molecular
Extruder Temperature (°C) 200 chain within the semi-crystalline materials has high mobility when
Build Plate Temperature (°C) 50 approaching its glass transition (Tg), between 60 °C and 80 °C
[18,19].
Ultimate tensile strength (UTS) for specimens exposed at 70 °C
did not have significant changes throughout the month ranging
from 46.16 MPa to 48.64 MPa. The tensile strength increased only
3.29% at 70 °C on 13rd day compared to the non-annealed speci-
men. However, the tensile strength then decreased until 31st day
at 46.16 MPa lower than non-annealed specimen which was at
47.09 MPa. As reported by many researchers, the different values
of stress were obtained due to the different brands of PLA filaments
used depending on their level of crystallinity and crystallization
behavior [20]. A study reported that the tensile strength for PLA-
PLUS increased only 2.87% at 80 °C compared with the non-
annealed specimen before it decreased [21]. Before annealed, the
tensile strength was 46.43 MPa, but after annealing at 80 °C, the
specimen recorded a slight increase at a value of 49.50 MPa.
Young’s modulus is referred to the gradient of the slope in the elas-
tic region [22]. The higher the modulus means the stiffer the mate-
rials it is. However, the brittleness of the specimen does not solely
depend on Young’s modulus as it is also affected by the strain. The
highest Young’s modulus is on the 24th day at 4.28 GPa but only
increased by about 14.13 % compared to the reference specimen
as shown in Fig. 5(b).
Fig. 4. Tensile testing load direction relative to the layer orientation of 3D printed For the heat treatment at 80 °C, a similar trend was observed for
PLA specimen. the stress–strain curve as the tensile strain value gradually
increased but in slight deviation until the 13rd day as shown in
Fig. 6(a). The maximum strain was also on the 13rd day at 4.54%.
the stress–strain curve for the temperature at 70 °C. When heat A team had reported that the threshold limit temperature for flex-
treatment or better known as annealing, was applied to the PLA ural strength was at 130 °C before the strength decreased about
specimens, the tensile strain increased from 3.01% (red-dotted line 15% when the temperature increased to 140 °C [23]. For the same
as a reference) up to 8.04% on the 13rd day. The reference speci- reason, it is proven that the optimum temperature for this type of
men was done at room temperature because the tensile testing filament is 70 °C compared to the specimens at 80 °C. Previous
was also done at this temperature. Then, the value of strain studies had shown that the improvement of mechanical perfor-
decrease significantly ranging from 3.55 to 3.60% after the 13rd mance of PLA was attributed from the increase of crystallinity

Fig. 5. (a) Tensile stress–strain curve at 70 °C; (b) Tensile strain (%) and Young’s modulus (GPa) vs number of exposure days at 70 °C.

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Ahmad Adnan Bin Abu Bakar, Muhammad Zulhilmi Bin Zainuddin, Ahmad Nurhelmy Bin Adam et al. Materials Today: Proceedings xxx (xxxx) xxx

Fig. 6. (a) Tensile stress–strain curve at 80 °C; (b) Tensile strain (%) and Young’s modulus (GPa) vs number of exposure days at 80 °C.

Fig. 7. (a) The stress–strain curve at room temperature; (b) Weight gain percentage (%) at room temperature.

when annealing was applied [12]. As PLA is well-known for its

behaviour as a slow crystallizing polymer [24], many strategies
have been adopted to figure out the ways to develop high crys-
tallinity in PLA including polymer blending and post-annealing in
order to increase its mechanical performance [25]. When the poly-
mer is treated with the heat treatment or changes its orientation of
layering, it will result in a quasi-amorphous state that eventually
promotes its ductility [26].
The ultimate tensile strength for temperature at 80 °C also did
not have significant changes throughout the month ranging from
43.55 MPa to 48.70 MPa. The highest Young’s modulus was
obtained on the 13rd day at 4.42 GPa. It is slightly higher than
the specimen at 70 °C as shown in Fig. 6(b). It is shown that higher
temperatures are also affecting Young’s modulus.
Contrary to the result of PLA printed materials under heat treat-
ment at 70 °C and 80 °C, the results of its tensile properties at room
temperature have shown poor tensile strain ranging from 2.06% to
3.90% and the ultimate tensile strength were ranging from
44.02 MPa until 48.08 MPa as shown in Fig. 7(a). This is likely to Fig. 8. Tensile strain (%) and Young’s modulus (GPa) vs number of exposure days at
be the effect of the PLA properties itself which is hygroscopic (ab- room temperature.

5
Ahmad Adnan Bin Abu Bakar, Muhammad Zulhilmi Bin Zainuddin, Ahmad Nurhelmy Bin Adam et al.
Fig. 9. (a) Tensile stress–strain curve under natural environment; (b) Tensile strain (%) and Young’s modulus (GPa) vs number of exposure days under natural environment.
sorb moisture) [27]. The results can also be proven by Fig. 7(b)
which shows the increase of weight ranging from 0.07% to 0.2%.
In the previous study, even though the 3D printed PLA specimens
were set to 100% infill, small gaps were created between each layer
[28]. Hence, creating the chances for the moisture to invade and
contributes to the poor bonding adhesion between the layer, thus
makes it more brittle. PLA is categorized as a class B polymer due to
its glass transition temperature (Tg) is above room temperature
and is typically brittle in behaviour [29]. Meanwhile, the Young’s
modulus at room temperature was almost consistent regardless
of the exposure days but slightly lowered compared with the spec-
imens placed at 70 °C and 80 °C as shown in Fig. 8.
As for the specimens that had been exposed directly under the
natural environment, the tensile strain obtained from this condi-
tion increases up to 10 days, then decreases as shown in Fig. 9
(a). The lowest tensile strain was on the 24th day at 1.98%. The
brittleness of the PLA specimens due to the direct exposure to sun-
light irradiation lead to the decrease of the tensile strain. In com-
parison, specimens that had been exposed directly to ultraviolet
radiation from sunlight would oxidize the molecular chain as sun-
light irradiation consists of high-energy photons [30]. This oxida-
Fig. 10. The tensile specimens under each condition; reference, at 70 °C, at 80 °C, at
23 °C (room temperature) and 32 °C (under natural environment); from left to right.
6
Materials Today: Proceedings xxx (xxxx) xxx
tion would eventually make PLA film less flexible and more
brittle when exposed under the xenon lamp [31]. According to
results obtained from differential scanning calorimetry (DSC), the
crystallinity of PLA nanocomposites increases after 60 days of
aging under natural weather [32]. The Young’s modulus for this
condition also did not have a significant impact as the values range
from 3.76 GPa until 4.13 GPa as shown in Fig. 9(b). The ultimate
tensile strength ranges between 46.51 MPa until 49.0 MPa.
Fig. 10 compares tensile specimens under each condition on the
13rd day and the reference specimen.
4. Conclusions
In the present study, the effect of post-heat treatment was
investigated on the mechanical property of the 3D printed Poly
(lactic acid) (PLA) by using fused deposition modelling process. It
was observed that:
 The different thermal treatment has considerable effect towards
the fracture limit of the structure, whilst minimal effect on the
tensile strength.
 The Young’s modulus for heat treatment above glass transition
is much higher than those below the glass transition.
 Post-processing annealing above glass transition promotes the
nucleation growth which increased crystallinity, thus promotes
the crystallinity of the 3D printed PLA crystalline fraction.
 Hence, it enhanced the Young’s modulus and ductility of the 3D
printed PLA. The Young’s modulus annealed at 80 °C increased
up to 18% whilst the strain increased almost three folded at
70 °C compared to the non-annealed 3D printed PLA.
 Mechanical brittleness is a common defect for PLA and became
a bottleneck for some applications, thus post-annealing with
optimum temperature could be an alternative way instead of
blending with other additive to enhance its mechanical
properties.
CRediT authorship contribution statement
Ahmad Adnan Bin Abu Bakar: Conceptualization, Methodol-
ogy, Writing – original draft, Visualization, Investigation. Muham-
mad Zulhilmi Bin Zainuddin: Conceptualization, Methodology,
Writing – original draft, Investigation. Ahmad Nurhelmy Bin
Adam: Methodology, Visualization, Investigation. Ikhwan Syafiq
Ahmad Adnan Bin Abu Bakar, Muhammad Zulhilmi Bin Zainuddin, Ahmad Nurhelmy Bin Adam et al.
Bin Mohd Noor: Supervision, Writing – review & editing, Formal
analysis. Nizam Bin Tamchek: Supervision, Writing – review &
editing, Formal analysis. Muhammad Syafiq Bin Alauddin: Writ-
ing – review & editing, Formal analysis. Mohd Ifwat Bin Mohd
Ghazali: Supervision, Resources, Writing – review & editing, Super-
vision, Project administration.
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
Acknowledgements
This research was supported by Ministry of Higher Education of
Malaysia (MOHE) through Fundamental Research Grant
Scheme (FRGS) with reference code, FRGS/1/2020/STG05/
USIM/02/1 and by Universiti Sains Islam Malaysia (USIM), grant
number (PPPI/COVID-19_0120/FST/051000/10320). This work
was carried out at Universiti Sains Islam Malaysia (USIM). The
authors would like to thank Muhammad Faishal Norjeli, Muham-
mad Afiq Hazizi Mahamood and Irfan Yahaya for their assistance
in collecting the data for this work. I would also like to thank our
lab assistants, Wan Shahrol Aznor Wan Osman and Mohd Zulkiflee
Mohd Zain for their guidance during this research.
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