Materials Circular Economy (2023) 5:10

https://doi.org/10.1007/s42824-023-00080-y

ORIGINAL PAPER

Prediction of Fibre Orientation in Biodegradable Composites

Reinforced With Short Date Palm Fibre Using Micromechanics
Modelling
Said Awad1 · Shafaat Ahmed Salahudeen2 · Lobna Elseify3 · Tamer Hamouda4 · Mohamad Midani3

Received: 1 May 2023 / Revised: 29 May 2023 / Accepted: 7 July 2023

© Crown 2023

Abstract
This study explores and evaluates a new micromechanical modelling to predict fibre orientation in biodegradable composite
reinforced with date palm fibre (DPF) using various DPF geometries. DPF/PLA composites were developed using compres-
sion moulding with four different reinforcement percentages (10, 20, 30, 40 wt.%) and four different fibre lengths (≤ 125,
125–250, 250–500, 500–1000) µm. Tensile strength and modulus of the composites were experimentally measured. The rule
of mixtures (ROM), inverse rule of mixture (IROM), modified ROM, modified IROM, and Halpin–Tsai were used with three
different fibre orientations scenarios in the composites to assess the efficacy of DPF orientations in the PLA. The predictions
demonstrate improvements over micromechanical models available in literature.

Keywords Natural Fibre Composite · Micromechanical Modelling · Biodegradable Composites · Modulus Prediction ·
Strength Prediction · Rule of Mixtures

Abbreviations Introduction
DPF Date palm fibre
PLA Polylactic acid The investigation of the utilization of biodegradable com-
NFPC Natural fibre-polymer composite posite for replacing non-biodegradable and petroleum-based
DPFRC Date palm fibre reinforced composite composites has been encouraged by the growing environ-
mental awareness and concerns as well as the scarcity of
natural resources (Dong et al. 2014; Siakeng et al. 2020).
Researchers have reported on the performance of a vari-
* Said Awad ety of biodegradable polymers (biopolymers), including,
said.awad@valorizen.com
polyhydroxyalkanoates (PHA), polylactic acid (PLA), and
Shafaat Ahmed Salahudeen polybutylene succinate (PBS) to be utilised as a matrix
shafaatht@gmail.com
system to produce biodegradable composites (Huda et al.
Lobna Elseify 2008; Foruzanmehr et al. 2016). These biopolymers can be
lobna.elseify@gmail.com
combined with other naturally occurring substances, such
Tamer Hamouda as natural plant fibres (NFs), to develop biodegradable com-
tehamoud@ncsu.edu
posites with improved properties (Jiao and Xiong 2014).
Mohamad Midani PLA is the most utilised biopolymer out of those that have
msmidani@ncsu.edu
been discussed (Martín del Campo et al. 2022). However,
1
Valorizen Research and Innovation Center, in contrast to synthetic or polymers made from petroleum,
Cairo Governorate, Egypt such as polyethylene and polypropylene, which cost between
2
Jazaa Energy Project India, No.1 Dawood Shahib St., 1.30 and 1.70 $/kg, biopolymers (such as PLA, which range
Chintadripet, Chennai, Tamil Nadu 600002, India in price from 2.50 to 3.20 $/kg) do not compel industries to
3
Materials Engineering Department, German University use them unless they are legally required to.
of Cairo, Al Tagamoa, Cairo Governorate, Egypt The agricultural sectors produce vast amounts of agro-
4
Textile Research Division, National Research Centre, waste each year. Globally, the poorly managed lignocel-
Cairo 12622, Egypt lulosic residues alone amount to more than 600 million

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tonnes/year. Recycling NF by incorporating them into
composites to manufacture renewable and biodegradable
materials has drawn significant attention as a biodegrad-
able reinforcing material (Elseify et al. 2019) due to a
number of factors, including low cost, biodegradability,
low density, availability, relative non-abrasiveness, and
lack of associated health hazards (Herrera-Franco and
Valadez-González 2004; Awad et al. 2020). They can also
help reduce waste and bring down the price of the compos-
ites that are created. It is likely that some plant fibres are
preferred and more cultivated in each region over others.
Date palm fibres (DPFs) are regarded as the region’s most
plentiful source of agricultural biomass waste, producing
more than 2.8 million tonnes a year (Elseify et al. 2019;
Awad et al. 2020). This waste is either burned or dumped
in landfills, which severely pollutes the environment and
kills vital soil microorganisms (Awad et al. 2020). Inves-
tigating an industrial use for this vast amount of biomass
waste is thus possible within the framework of waste
management programmes already in place in most of the
world’s nations. The utilization of DPF does create issues,
as it does with all NF. Due to the hydrophilic character
of lignocellulosic fibres, it is difficult to acquire adequate
adhesion to hydrophobic polymers. This is because there
are lots of hydroxyl groups on the fibre, which give it a
strong affinity for water and make it difficult for non-polar
polymers to properly wet the fibres. Several experiments
have been done to improve the compatibility of natural
fibres with polymers. This was successfully accomplished
by either treating the DPF chemically or physically (Ami-
rou et al. 2013; Lahouioui et al. 2020; Awad et al. 2022)
or, as described by multiple researchers, by utilising cou-
pling agents, which increase the adhesion between the NF
and polymer matrix (Matuana et al. 1998; Mittal et al.
2016). However, a crucial component of comprehending
the geometry, diameter and length, of NF and in particular
DPF, has not yet been thoroughly investigated by micro-
mechanical, and there is a lack of agreement on how these
parameters affect their effectiveness as a reinforcement in
polymeric composites. It was noticeable in many research
utilizing NF with polymer matrices is that the experimen-
tal values are different than the theoretical values. Several
reasons contribute towards this phenomenon such as the
fibre content, fibre interfacial bonding and fibre geometry
(aspect ratio). The increase in NF percentage makes the
composite stiffer and failure strain reduces which affects
the prediction accuracy (Abhilash et al. 2021). Fibre pull-
out from the matrix creates crack at the matrix interface
that enhances the composite mechanical rate of failure
(Facca et al. 2007). Moreover, improper adhesion at the
matrix/fibres interface provides less experimental results
due to low adhesion between the hydrophilic natural
fibres and the hydrophobic polymer matrix (Dittenber
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Materials Circular Economy (2023) 5:10
and Gangarao 2012). Furthermore, fibre orientation in the
matrix due to melt flow affects the predicted mechanical
properties of the composite (Cordin et al. 2018).
Mechanical test devices and surface analysis tools are
typically used to evaluate natural fibre-polymer composite
(NFPC) properties. These factors combined helped us fully
comprehend the NFPC’s mechanical characteristics, water
absorption abilities, durability, and other characteristics. In
recent years, some researchers have widened their research
methodology by utilising mathematical models to forecast
the characteristics of NFPC. The most popular and well-
known theories for describing mechanical properties are the
rule of mixtures (ROM), inverse ROM (IROM), Cox model,
Hirsch model, Halpin–Tsai model, Bowyer-Bader model,
and Kelly-Tyson model. A simple and effective method for
understanding and predicting the behaviour of a composite
based on the properties of its constituent parts is analytical
modelling. These hypotheses have been made in an effort to
model the mathematical various characteristics of composite
materials (Cao et al. 2014). However, compared to other
composites, very little mathematical analytical methodology
is used in NFPC research.
In general, NFPC show enhanced properties in the fibre
oriented direction such as high tensile strength and mod-
ulus (Wazzan 2005; Gao and Yang 2019). Fibre orienta-
tion in moulded thermoplastic parts is caused by melt flow
(McNally 1977). Though there are numerous studies which
focused on the micromechanical modelling of natural fibre
(Facca et al. 2007; Virk et al. 2012; Cordin et al. 2018;
Salahudeen 2020), this study is considered as the first for
presenting a micromechanical model for prediction of fibre
orientation in the matrix using the tensile and flexural modu-
lus of DPF reinforced biodegradable thermoplastic, PLA,
composites. The model presented in the research explores
the way to identify the orientation of short fibres prepared
using compression moulded and addresses the statistical
variation in DPF reinforcement of different sieve size and
content in biodegradable composites. In general, this study
provides research methodology to predict the fibre orienta-
tion in all the fibre composite.
Materials and Methods
Materials
The raw DPF, sometimes referred to as DPF sheath or mesh,
that encircles the stems of date palm trees was provided
by Egypt’s Valorizen Research and Innovation Center. To
clear the surface of the fibres of dust and grime, DPFs were
washed in distilled water. To make sure the fibres had a low
moisture content, the DPFs were then dried in a vacuum
oven at 60 °C for 24 h. Afterwards, fibres were ground using
Materials Circular Economy (2023) 5:10
a German Retsch cutting mill (SM 100), fitted with a 2 mm
sieve. The grinded DPF was sieved through different mesh
sizes of 125 µm, 250 µm, 500 µm and 1000 µm using an
automatic sieving machine, and the fibres that were main-
tained on each screen were kept in sealed polythene bags
to prevent any moisture absorption from the environment.
Moreover, PLA and polymer matrix were purchased in pel-
let form from Ecodeck Ltd., a top composite manufacturing
business in the UK. In order to guarantee that the polymer
had a low moisture content, the pellets were dried in an oven
at 60 °C for 24 h.
Processing of Composites
With a Brabender Plastograph twin-screw mixer (with Cam
blades for mixer type N50EHT) at 50 rpm for 10 min, the
DPF and polymer matrix, PLA, were treated. For composites
created utilising PLA as a polymer matrix, the temperature
of the Brabender was 170 °C. Four different mass propor-
tions and four different fibre diameter sizes of samples were
created. This was done by adding the necessary amount of
polymer for each batch into the mixer at first, letting it melt
Fig. 1  PLA reinforced date palm fibre composite development
Page 3 of 13 10
completely for three minutes, and then adding the DPF to
create a homogenous mixture over the course of seven min-
utes. The resulting mixture was then processed through a
Retsch cutting mill (SM 100, Germany) fitted with a 2 mm
sieve to produce pellets. Using an electrically heated hydrau-
lic press, the ground pellets were compression moulded into
a 100 mm (L) × 100 mm (W) × 4 mm (T) mould. The com-
pression moulding process entailed preheating the mould
at 170 °C for 10 min without any load, compressing it for
5 min at that temperature under 10 MPa pressure, and then
cooling it till it reached 35 °C while still under stress. Using
a SEALEY SM1304 band saw, the compression moulded
composite was cut into 100 mm (L) × 10 mm (W) × 4 mm
(T) samples for testing its physical and mechanical proper-
ties (Fig. 1).
Mechanical Property Analysis
Flexural Strength Test
Using an Instron 5900 testing machine with a load cell
capacity of 30 kN and a speed of 1 mm/min, the flexural
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 10 Page 4 of 13 Materials Circular Economy (2023) 5:10

properties of the produced composites were tested at 25 °C

and relative humidity of 60% calculated in accordance with
BS EN ISO 14125:1998. The flexural characteristics were
measured using three-point bending.

Tensile Strength Test

According to BS EN ISO 527–2:2012, the produced com-

posites’ tensile strength properties were evaluated at 25 °C
and 60% relative humidity. An Instron 5900 testing device
with a load cell capacity of 30 kN and a speed of 1 mm/min
was used for the test.
Five samples were tested and at least four replicate sam-
ples have been presented as an average value of tested sam-
ples for both the flexural and tensile strength tests.

Micromechanical Models
Micromechanics is the study of materials down to their
smallest components. In micromechanical modelling of
composites, macroscopic behaviour of the composite is pre-
dicted based on the behaviour of its constituents.
Rule of mixture (ROM) states that a composite’s proper-
ties are equal to the total of the volume-weighed properties
of its constituent materials, meaning that both phases of the
material are subject to the same strain when under stress.
ROM, termed as ­ROMP, serves as the upper bound for the
composite modulus (Ibrahim et al. 2014);
( )
E1 = EF VF + EM VM (1)
where ­E1 is the elastic modulus of the composite in fibre
direction, ­EF is the elastic modulus of the fibre, ­EM is the
elastic modulus of the matrix, ­VM is the volume fraction
of matrix and ­VF is the volume fraction of Fiber. VF can be
calculated using Eq. (2) (Abhilash et al. 2021):
⎛ WF ⎞ sidered to be 1; for fibres oriented in two directions at right
⎜ ρF ⎟ angles (cross-laid fibres or bi-directional), when stress is in
VF = ⎜ � � � � ⎟ (2)
⎜ WF WM
+ ρ ⎟
⎝ ρF M ⎠
Fig. 2  SEM image of cellular structure of DPF (Awad et al. 2021)
where WF and WM is the weight fraction of the fibre
and matrix, ρF and ρM is the density of fibre and matrix,
respectively.
In moulded composite parts, the orientation of fibre plays
a very important role in the mechanical properties that can
be achieved. Contribution of fibre reinforcement to the mod-
ulus of the composite depends mainly on its orientation.
Fibres provide maximum stiffness when it is aligned along
the direction of loading. To account for the alignment of
fibres, a fibre orientation factor (K) can be introduced into
ROM, Eq. (1), and termed Eq. (2) as modified ­ROMP (Osoka
Emmanuel 2018);
( )
E1 = KEF VF + EM VM (3)
Values of k depend on how the fibre is oriented; for per-
fect alignment, when stress is parallel to the fibres, K is con-
one of these directions, K is considered to be 0.5; for fibres
randomly and uniformly distributed within a specific plane,
when stress is in any direction in the plane of the fibres,

Table 1  Volume of fraction and Material Density (g/cm3) 10% DPF 20% DPF 30% DPF 40% DPF
volume of voids for DPF/PLA wt % wt % wt % wt %
composite with different DPF
content and size Vf Vv Vf Vv Vf Vv Vf Vv

PLA 1.178 - - - - - - - -
≤ 125 µm DPF 0.4079 0.24 0.11 0.42 0.18 0.55 0.24 0.66 0.40
125–250 µm DPF 0.5024 0.21 0.07 0.37 0.15 0.50 0.18 0.61 0.31
250–500 µm DPF 0.4762 0.22 0.09 0.38 0.16 0.51 0.20 0.62 0.29
500–1000 µm DPF 0.4413 0.23 0.10 0.40 0.19 0.53 0.24 0.64 0.31

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Materials Circular Economy (2023) 5:10 Page 5 of 13 10

Fig. 3  Schematic demonstration

of DPF aligned in the direction
of tensile force

K = 0.375; and for fibres randomly and uniformly distributed where ­E2 is the composite modulus, in a direction transverse
within three dimensions in space and stress is in any direc- to the fibres.
tion (K = 0.2). In 1929, using the inverse ROM “Reuss” pre- Modified IROM models for composite modulus, in a
dicted the lower bound properties of composite reinforced direction transverse to the fibres, are also presented by Voyi-
with fibre. When the composite is loaded in a direction trans- adjis and Kattan (Voyiadjis and Kattan 2005);
verse to the fibres, both the fibres and the matrix suffer the
same stress. This phenomenon is known as the inverse rule ⎛ ⎞
⎜ V + 𝜂V ⎟
of mixture (IROM) or ROMS (Ibrahim et al. 2014);
E2 = ⎜ � F� � M � ⎟ (5)
( ) ⎜ VF 𝜂V ⎟
EF EM ⎜ E + EM ⎟
E2 = (4) ⎝ F 2 M ⎠
EF Vm + EM VF

5 5

4.5 4.5

4 4
Young's Modulus (GPa)

Young's Modulus (GPa)

Exp. ≤125
3.5 3.5 Exp.250-500

K=0.2
3 3 K=0.2
K=0.375
2.5 2.5 K=0.375
K=0.5
2
2
ROM K=1 K=0.5
1.5
1.5
Halpin-Tsai ROM K=1
1
1
0.5 Halpin-Tsai
0.5
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0
Vf of DPF 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7
Vf of DPF

Fig. 4  ROM, modified ROM and Halpin–Tsai model compared with

experimental results at DPF size ≤ 125 µm Fig. 6  ROM, modified ROM and Halpin–Tsai model compared with
experimental results at DPF size 250–500 µm
5
4.5
4.5
4
4
Young's Modulus (GPa)

3.5
Young's Modulus (GPa)

3.5 Exp.125-250
Exp. 500-1000
3
3
K=0.2
2.5 K=0.2
2.5
K=0.375
2 2 K=0.375
K=0.5
1.5 1.5 K=0.5
ROM K=1
1 1 ROM K=1
Halpin-Tsai
0.5 0.5 Halpin-Tsai
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7
Vf of DPF Vf of DPF

Fig. 5  ROM, modified ROM and Halpin–Tsai model compared with Fig. 7  ROM, modified ROM and Halpin–Tsai model compared with
experimental results at DPF size 125–250 µm experimental results at DPF size 500–1000 µm

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 10 Page 6 of 13 Materials Circular Economy (2023) 5:10

Table 2  ROM, modified ROM and Halpin–Tsai model compared with experimental results using numerical model 1
Composition DPF size Young’s modulus ROM (K = 1) ROM (K = 0.2) ROM (K = 0.375) ROM (K = 0.5) Halpin–Tsai
Є = 2(L/D)
(Wt. %) (µm) (GPa)

Pure PLA - 2.757 2.757 2.757 2.757 2.757 2.757

90/10 PLA/DPF ≤ 125 1.550 3.302 2.33 2.543 2.695 3.22
125–250 1.620 3.221 2.394 2.575 2.704 3.165
250–500 1.250 3.241 2.378 2.567 2.702 3.207
500–1000 1.688 3.27 2.355 2.555 2.698 3.251
80/20 PLA/DPF ≤ 125 1.355 3.697 2.020 2.387 2.649 3.586
125–250 1.375 3.586 2.108 2.431 2.662 3.505
250–500 1.355 3.614 2.086 2.42 2.659 3.566
500–1000 1.488 3.655 2.054 2.404 2.654 3.628
70/30 PLA/DPF ≤ 125 1.295 3.998 1.785 2.269 2.615 3.881
125–250 1.328 3.881 1.876 2.315 2.628 3.793
250–500 1.420 3.911 1.853 2.303 2.625 3.86
500–1000 1.350 3.954 1.819 2.286 2.62 3.926
60/40 PLA/DPF ≤ 125 1.075 4.233 1.601 2.176 2.588 4.125
125–250 1.188 4.125 1.685 2.219 2.6 4.039
250–500 1.250 4.153 1.663 2.208 2.597 4.105
500–1000 1.190 4.193 1.632 2.192 2.592 4.167

where ƞ is the stress-partitioning factor and EF2 is fibre where ζ is a shape parameter depending on the filler geom-
modulus in the transverse direction. ƞ satisfies the condi- etry and loading direction. Є = 2 (L/D) for fibres (Affdl and
tion 0 < ƞ < 1, but usually taken between 0.4 and 0.6. Thus, Kardos 1976). For transverse direction, Є = 2 (constant) is
ƞ values considered in this study are 0.4, 0.5 and 0.6. considered for all composites.
The “Halpin–Tsai” model illustrates the relationship
between filler aspect ratio and volume fraction and the influ-
Microstructure Analysis
ence of fibre reinforcing on the stiffness characteristics of
composite. Equation (6) represents the elastic modulus of a
The microstructure of the composites developed where ana-
composite material in the Halpin–Tsai model.
lysed to ensure the homogenous combination between the
( )
1 + 𝜁𝜂VF polymer, PLA, and NF, DPF, which was examined using
EC = EM (6) a scanning electron microscope (SEM), TESCAN-VEGA
1 − 𝜂VF
3 (Czech Republic) field emission, as well as the failure
( ) mechanism due to various sieving sizes. The samples were
EF − EM
∁ ⪯= (7) prepared by adhering them to carbon adhesive tape. To add
EF + 𝜁 ∗ EM electrical conductivity, the samples were coated with a thin
gold film using an Edwards S 150B sputter coater. After
( )
L coating, samples were examined and used in an Energy
ζ=2 (8)
D Dispersive X-rays (EDX) analyser machine with a 30 kV
coupling.

Fig. 8  Schematic demonstration of DPF aligned perpendicular to tensile force

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Materials Circular Economy (2023) 5:10 Page 7 of 13 10

5.0 5.0

4.5 4.5

4.0 4.0
Young's Modulus (GPa)

Young's Modulus (GPa)

Exp.250-500
Exp. ≤125
3.5 3.5
n=0.4
3.0 n=0.4 3.0
2.5 2.5 n=0.5
n=0.5
2.0 2.0
n=0.6 n=0.6
1.5 1.5
IROM IROM
1.0 1.0
Halpin-Tsai
0.5 0.5 Halpin-Tsai

0.0 0.0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7
Vf of DPF Vf of DPF

Fig. 9  IROM, modified IROM and Halpin–Tsai model compared Fig. 11  IROM, modified IROM and Halpin–Tsai model compared
with experimental results at DPF size ≤ 125 µm with experimental results at DPF size 250–500 µm

Results and Discussion
Adding short fibres to a polymer matrix is typically done to
enhance the composite’s mechanical properties. It is highly
intriguing and merits further investigation that the addition
of fibre in this study causes a decline in the overall perfor-
mance of the polymer matrix. This phenomenon is due to the
utilization of untreated DPF which forms a weak interfacial
bonding with PLA, due to their hydrophilic characteristics.
Micromechanics modelling of composite is carried out uti-
lising Halpin-Tasai Equations, modified inverse rule of mix-
ture, inverse rule of mixture, and rule of mixture in order to
determine the cause.
Using Eq. (2), the volume fraction ­(Vf) of the fibre and
matrix was determined. Using the density of the composites
as shown in Table 1, the void fraction ­(Vv) of the composites
was evaluated. A scanning electron microscope image of a
single cross-sectional DPF is used to demonstrate the cel-
lular structure of DPF as shown in Fig. 2. Using the tensile
strength test and flexural strength, the Young’s modulus and
flexural modulus of the composites were determined from
the compression moulded samples. The DPF is considered to
have a Young’s modulus of 5 GPa based on previous attempt
done by the same group of researchers (Awad et al. 2020).
DPF Aligned in Direction of Tensile Force (Numerical
Model 1)
A schematic diagram that demonstrates numerical model 1
scenario where all short DPFs are in an iso-strain condition
for Young’s modulus, which means they are oriented in the
direction of the tensile force shown in Fig. 3. Strain in the
fibre, matrix, and composite are all assumed equal when the
fibre-aligned composite is loaded in the fibre alignment’s
longitudinal direction.
Numerical model 1 calculation was performed using
ROM Eq. (1), modified ROM Eq. (3), and Halpin–Tsai
Eq. (6) for four different fibre sizes ≤ 125 µm, 125–250 µm,
250–500 µm, and 500–1000 µm. Young’s modulus value of

5.0 5.0
4.5 4.5
4.0 4.0
Young's Modulus (GPa)

Young's Modulus (GPa)

Exp.125-250
3.5 Exp. 500-
3.5
1000
n=0.4
3.0 3.0 n=0.4

2.5 n=0.5 2.5 n=0.5

2.0 n=0.6 2.0

n=0.6
1.5 1.5
IROM IROM
1.0 1.0
Halpin-Tsai Halpin-Tsai
0.5 0.5
0.0 0.0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7
Vf of DPF Vf of DPF

Fig. 10  IROM, modified IROM and Halpin–Tsai model compared Fig. 12  IROM, modified IROM and Halpin–Tsai model compared
with experimental results at DPF size 125–250 µm with experimental results at DPF size 500–1000 µm

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 10 Page 8 of 13 Materials Circular Economy (2023) 5:10

Table 3  IROM, modified IROM and Halpin–Tsai model compared with experimental results using numerical model 2
Composition DPF size Young’s modulus IROM Modified IROM Modified IROM Modified IROM Hal-
(n = 0.4) (n = 0.5) (n = 0.6) pin–Tsai
(Є = 2)
(Wt. %) (µm) (GPa)

Pure PLA - 2.757 2.757 2.757 2.757 2.757 2.757

90/10 PLA/DPF ≤ 125 1.550 3.094 1.547 1.635 1.710 3.209
125–250 1.620 3.039 1.628 1.721 1.800 3.139
250–500 1.250 3.052 1.607 1.698 1.776 3.156
500–1000 1.688 3.072 1.577 1.667 1.743 3.181
80/20 PLA/DPF ≤ 125 1.355 3.396 1.294 1.353 1.407 3.570
125–250 1.375 3.305 1.349 1.415 1.476 3.465
250–500 1.355 3.327 1.334 1.398 1.457 3.491
500–1000 1.488 3.360 1.314 1.376 1.432 3.529
70/30 PLA/DPF ≤ 125 1.295 3.667 1.184 1.225 1.263 3.864
125–250 1.328 3.557 1.222 1.269 1.313 3.747
250–500 1.420 3.584 1.212 1.257 1.299 3.777
500–1000 1.350 3.625 1.198 1.240 1.281 3.819
60/40 PLA/DPF ≤ 125 1.075 3.912 1.123 1.151 1.178 4.108
125–250 1.188 3.795 1.149 1.183 1.215 3.994
250–500 1.250 3.825 1.142 1.174 1.205 4.024
500–1000 1.190 3.868 1.132 1.163 1.191 4.065

the tensile test results was considered as the experimental
data.
Elastic modulus of the composite is shown in Figs. 4, 5, 6,
and 7 at various DPF ­Vf and with different DPF diameters.
The numerical model 1 values exceeded all experimental
findings, which amply demonstrates that the fibres are not
aligned and oriented in the direction of tensile loading. As
shown in Table 2, misaligned DPF had a negative effect on
the composite’s overall elastic modulus where the addition
of DPF reduced the over strength of the composite.
Based on the V f and elastic modulus of the com-
posites developed, ROM provide the upper bound of
the elastic modulus of composites as demonstrated in
Table 1. The highest achievable modulus is provided
by ROM assuming that the reinforcement is aligned in
the direction of the force and continuous. The results
showed that the modulus predicted by ROM is greater
than experimental values because ROM disregards
the inhomogeneity brought on by the shape, orienta-
tion and size of short DPF. Composites reinforced with
short DPF are always thought of as having an elastic
modulus that is no greater than ROM. Moreover, ROM
ignores the random orientation distribution of DPF,
which directly affects the composites’ modulus. The
larger packaging of DPF within the same volume can
also be explained by the fact that PLA/DPF composites
developed demonstrated an increase in modulus as the
amount of DPF rose. It can be assumed that the DPF
were oriented roughly perpendicular to the direction of
the tensile force and that this is why the experimental
results were close to modified ROM with K = 0.2. The
variance was the least between the rest of the assump-
tions taken into consideration, ranging between 30
and 90%. This is because the DPF were distributed

Fig. 13  Schematic demonstra-

tion of DPF aligned in direction
of flexural force

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Materials Circular Economy (2023) 5:10 Page 9 of 13 10

6 6
5.5 5.5
5 5
Exp. ≤125

Flexural modulus (GPa)

Flexural modulus (GPa)

Exp.250-500
4.5 4.5
4 K=0.2 4
K=0.2
3.5 3.5
K=0.375
3 3 K=0.375
2.5 K=0.5 2.5
2 K=0.5
2
1.5 ROM K=1 1.5
ROM K=1
1 1
Halpin-Tsai
0.5 0.5 Halpin-Tsai
0 0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7
Vf of DPF Vf of DPF

Fig. 14  ROM, modified ROM and Halpin–Tsai model compared with Fig. 16  Comparison of ROM, modified ROM and Halpin–Tsai model
experimental results at DPF size ≤ 125 µm with experimental results at DPF size 250–500 µm

non-uniformly and randomly throughout three dimen-
sions in the composite. DPF with the highest geometry
size (500–1000 µm) showed the least variance when
compared to the experimental results when the load-
ing content was high (30–40 wt.%) but at lower fibre
content (10–20 wt.%) DPF geometry with 250–500 µm
showed the least variance when compared to the experi-
mental results. ROM (K = 1) and Halpin–Tsai showed
almost the same variance when compared to the experi-
mental results ranging between 93 and 294%.
DPF Aligned Perpendicular to Tensile Force
(Numerical Model 2)
Numerical model 2 scenario, where all short DPFs are
aligned in the direction of the compression force, is sche-
matically demonstrated in Fig. 8. Assuming that the DPF are
normal to the direction of the tensile testing, or the iso-stress
condition for Young’s modulus, test samples were made
from 4 mm compression moulded sheet. Stress in the fibre,
matrix, and composite are all treated equally when loading a
fibre-oriented composite in the transverse direction of fibre
alignment. To apply the rule of mixture to this numerical
model 2, IROM must be adjusted.
Numerical model 2 calculation was performed using
IROM Eq. (4), which gives the lower bound of elastic
modulus of composites. Modified IROM, Eq. (5), and Hal-
pin–Tsai, Eq. (6), for four different fibre sizes ≤ 125 µm,
125–250 µm, 250–500 µm, and 500–1000 µm. The results
of the tensile test’s Young’s modulus value were used as the
experimental data. To fit the numerical curve in Eq. (6), the
Young’s modulus of fibre in the transverse direction is taken
to be 1 GPa. This has been assumed that 1/5 of the strength
of DPF is taken into consideration due to the fibre not being
in the direction of the force, weak interfacial bonding, and
being short fibres (Ibrahim et al. 2014).
Figures 9, 10, 11, and 12 display the composite’s elastic
modulus at various DPF ­Vf and four distinct fibre diam-
eters. According to Table 3, the numerical model 2, values
for the IROM and Halpin–Tsai models were greater than
the outcomes of the experiments. According to the numeri-
cal curve that is synchronised with the experimental curve

6 6

5.5 5.5
5 Exp.
5 500-10...
Flexural modulus (GPa)

Exp.125-250
Flexural modulus (GPa)

4.5 4.5
K=0.2
4 4
K=0.2
3.5 3.5 K=0.375

3 K=0.375 3
K=0.5
2.5 2.5
K=0.5 2
2 ROM K=1
1.5 1.5
ROM K=1
1 1 Halpin-T...

0.5 Halpin-Tsai 0.5

0 0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7
Vf of DPF Vf of DPF

Fig. 15  ROM, modified ROM and Halpin–Tsai model compared with Fig. 17  Comparison of ROM, modified ROM and Halpin–Tsai model
experimental results at DPF size 125–250 µm with experimental results at DPF size 500–1000 µm

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 10 Page 10 of 13 Materials Circular Economy (2023) 5:10

Table 4  Halpin–Tsai model, modified ROM model, and the ROM model compared with experimental results using numerical model 3
Composition DPF size Flexural modulus ROM (K = 1) ROM (K = 0.2) ROM (K = 0.375) ROM (K = 0.5) Halpin–Tsai
Є = 2(L/D)
(Wt. %) (µm) (GPa)

Pure PLA 3.306 3.306 3.306 3.306 3.306 3.306

90/10 PLA/DPF ≤ 125 3.221 3.717 2.746 2.958 3.110 3.676
125–250 3.402 3.656 2.829 3.010 3.139 3.629
250–500 3.355 3.671 2.809 2.997 3.132 3.655
500–1000 3.522 3.694 2.778 2.979 3.122 3.684
80/20 PLA/DPF ≤ 125 3.211 4.016 2.339 2.706 2.968 3.961
125–250 3.500 3.932 2.454 2.777 3.008 3.892
250–500 3.111 3.953 2.425 2.759 2.998 3.930
500–1000 3.855 3.984 2.383 2.733 2.983 3.971
70/30 PLA/DPF ≤ 125 3.033 4.243 2.031 2.515 2.860 4.185
125–250 3.700 4.155 2.150 2.589 2.902 4.112
250–500 3.086 4.178 2.119 2.570 2.891 4.153
500–1000 3.840 4.210 2.076 2.542 2.876 4.197
60/40 PLA/DPF ≤ 125 2.700 4.421 1.788 2.364 2.775 4.368
125–250 3.100 4.339 1.900 2.433 2.814 4.297
250–500 2.900 4.361 1.871 2.415 2.804 4.337
500–1000 2.850 4.390 1.830 2.390 2.790 4.378

in the modified IROM model Eq. (5), DPF fibre contributes
around 20% to the overall performance of the composite
when the elastic modulus of the fibre E
­ F2 is at 1 GPa. The
total findings demonstrated that fibres are more inclined
to point in a transverse direction as opposed to an axial
direction.
For transverse loading, an equal tension is assumed
at the fibre and the matrix. The premise of equal stress
is no longer true for the composite because each com-
ponent experienced a different stress when the fibres
were inclined. The mixing Eq. 5’s typical inverse rule
is achieved when n = 1. Typically, n between 0.4 and
0.6 is considered for elastic zones, and it correlates
well with the results of the experiments, as shown in
Table 3 and Figs. 9, 10, 11, and 12. The conclusion
shows that the fibres were transverse to the direction
of the tensile force. Results further support numerical
model 2 and demonstrate that fibres are aligned perpen-
dicular to the direction of tensile tension. Comparing
numerical model 2 to the experimental results, using
IROM with (n = 0.4, 0.5, and 0.6), the variance between
the model and the experimental results was in a range
of ± 42%. Excluding the results of DPF content 10 wt.%
of fibre size 250–500 µm, the variance drops to ± 15%.
This proves that the DPF where transverse to the direc-
tion of the tensile force. Furthermore, as the value of n
increased from 0.4 to 0.6, the model predication became
close to the experimental values and the variance dif-
ference decreased.
DPF Aligned in Direction of Flexural Force
(Numerical Model 3)
In theory, the intensity of DPF along the fibre direc-
tion will be greater than the other directions if they are
positioned at an angle. Figure 13 provides a schematic
illustration of the numerical model 3 scenario where all
short fibres are aligned with the direction of the com-
pression force to validate numerical model 3. Accord-
ing to the “Processing of Composites” section, the tested
samples were made from 4 mm compression moulded
sheet, and it was assumed that the DPF would be aligned
with the direction of the flexural strength test, or the
iso-strain condition for flexural modulus. Strain in the
DPF, matrix, and composite are all treated equally when
the DPF-oriented composite is loaded in the longitudinal
direction of DPF alignment.
For four distinct DPF sizes ≤ 125 µm, 125–250 µm,
250–500 µm, and 500–1000 µm numerical calculations
were made using ROM Eq. (1), modified ROM Eq. (3), and
Halpin–Tsai Eq. (6). The findings of the flexural strength
test were used to calculate the flexural modulus. Also, it is
worth noting that isotropic materials like polymers, flexural
modulus of elasticity is equivalent to the tensile modulus
(Young’s modulus) of elasticity.
Elastic modulus of the composite is shown in Figs. 14, 15, 16,
and 17 at various DPF volume fractions and with four distinct
fibre diameters. All experimental findings fall within the theo-
retical range of ROM (K = 1) to ROM (K = 0.5), which amply

13
Materials Circular Economy (2023) 5:10 Page 11 of 13 10

Fig. 18  Microstructure of PLA

composite reinforced with
different DPF geometry and
content. A (500 - 1000 µm DPF
with 10 wt.%), B (250 - 500 µm
with 30 wt.%), C (125 - 250 µm
with 20 wt.%), D (≤ 125 µm
DPF with 10 wt.%)

demonstrates that fibres are orientated between 0° and 45° in the
direction of flexural loading. Also, it demonstrates that in sam-
ples produced via compression moulding, short fibres were more
likely to align in the force’s direction. The outcome demonstrates
that an improvement in mechanical property performance can
be anticipated in the direction of compression moulding. No
matter how long the short fibre DPF is, all numerical modelling
produces results that are comparable to the experimental DPF/
PLA composite findings. The results of this investigation are
only reported when the DPF length is less than or equal to the
thickness of the compression-moulded samples.
The results shown in Figs. 14, 15, 16, and 17 and in
Table 4 that the experimental results line up between K = 1
and K = 0.5 can be explained as follows: at K = 1, fibres are
oriented parallel to the stress (tensile or flexural force), and
at K = 0.5, they are oriented at a right angle to the direction
of applied stress. The results show that the stress is trans-
ferred from the matrix to the fibre at K = 1 and K = 0.5, and
most likely, the DPF are orientated between 0° and 45°. Fur-
thermore, the as the value of K increased from 0.2 to 0.5, the
model predication became close to the experimental values
and the variance difference decreased.
DPF Geometry’s Impact on the Composite’s
Microstructure
Figure 18 shows the SEM microstructure of PLA bio-
composite samples reinforced with different DPF diameter

13
 10 Page 12 of 13
size and ­Vf. Starting with the micro cellulose crystals and
progressing to the technical fibre bundles depicted in
Fig. 18 B, DPF has a hierarchical structure. The bundle
of elemental cellulose fibrils that make up the technical
fibre are joined by lignin and hemicellulose. The thick
walls and wide lumens of DPF fibrils produce the cellu-
lar structure within the bundle, as seen in Fig. 18C. The
technical fibre has a rough surface made up of hexagonal
scales, as seen in Fig. 18D. The interlocking mechanism
produced by the rough fibre surface nevertheless permits
loads to be transferred from the PLA matrix to the fibre
in spite of the poor compatibility level between the fibre
and the polymer. Smaller DPF sieve sizes improve load
transfer efficiency and reduce fibre pullouts by increasing
the surface area in contact with the PLA matrix. In con-
trast, as the fibre weight fraction is increased, voids begin
to form as a result of the high melt viscosity of PLA and
the difficulty of completely wetting the fibres, as seen in
Fig. 18C. Due to the weak interfacial strength, Fig. 18A
shows how under loading causes the fibre to flex elasti-
cally until it separates from the matrix, while Fig. 17B
shows how additional loading causes the debonding front
to spread until the fibre is totally pulled out.
Conclusion
This study offered a method for predicting the orientation
of DPF arranged in a thermoplastic matrix created by com-
pression moulding a PLA composite reinforced with DPF
and comparing it to experimental results, which is the main
goal of any research focusing on composites. For short natu-
ral fibres, the orientation of the fibres in the compression
moulding process should be similar to that of the injection
moulding. Also, based on the type of applications for short
natural fibres, this result aids researchers in selecting the
sample preparation technique. To a great extent, results are
valid to short NF. Numerical model 1 demonstrated that the
results differed from the experimental findings because the
DPF was not oriented in the direction of the tensile force.
According to numerical model 2, DPF only contributed 20%
of its modulus to the PLA reinforced DPF composite, and
the fibres were aligned perpendicular to the direction of the
tensile stress. Numerical model 3 demonstrated the correla-
tion between numerical simulation and experimental find-
ings and established that DPF is directed between 0° and 45°
in the direction of compression melt flow. The development
of short DPF composites employing injection moulding
and replication of this approach of analysis can be done in
the future to define the numerical relationship more clearly
between fibre orientation and short fibre DPF composites.
13
Materials Circular Economy (2023) 5:10
Author Contribution Said Awad—conceptualized, experimental and
model work, and writing the first draft; Ahmed Salahudeen—con-
ceptualized and model work; Lobna Elseify—experimental work and
assisted in the writeup of the first draft; Tamer Hamouda—conceptu-
alized and data curation; Mohamad Midani—reviewed, detailed the
manuscript, and supervision.
Data Availability The datasets used and/or analysed during the cur-
rent study are available from the corresponding author on reasonable
request.
Declarations
Competing Interests The authors declare no competing interests.
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