Biomass Conversion and Biorefinery (2024) 14:9897–9913

https://doi.org/10.1007/s13399-024-05431-6

ORIGINAL ARTICLE

Durability evaluation of treated pineapple leaf biopolymer composites

for enhanced eco‑friendly mortar towards sustainability
Bebitta Robinson Chellathurai1 · Ninija Merina Rymond1

Received: 22 January 2024 / Revised: 7 February 2024 / Accepted: 8 February 2024 / Published online: 24 February 2024
© The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature 2024

Abstract
The present work aimed to investigate the prospect of reusing natural fibers obtained from pineapples as a reinforcing ele-
ment in eco-friendly mortar exploring physical, morphological, and chemical characteristics of natural fibers in untreated
and treated conditions using sodium hydroxide (NaOH) for building materials. Also, the technological properties of mortars
in fresh state, including setting time, drying shrinkage, and sorptivity were assessed. In addition, extensive research was
conducted on solidification stage of mortars, which includes durability, flexural, and compression test. The results revealed
that treating fiber with 6% NaOH enhanced the fiber properties, and incorporation of 2.5% treated fiber by mass of cement
resulted in improved technological and durability properties of mortar. Furthermore, this proposed novel approach not only
enhances the mechanical characteristics of mortar but also addresses the potential for utilizing natural fibers in cementitious
building materials thereby reducing environmental impacts.

Keywords Pineapple fiber · NaOH · Durability · Biocomposites · Building materials

1 Introduction synthetic fibers, and natural fibers is extensively employed

in the reinforcement of cementitious composites. Numerous
As per the recommendations of International Commission empirical investigations have provided substantial evidence
upon the Development of Environment, sustainability is supporting the notion that inclusion of synthetic fibers or
defined as the ability to meet present needs while ensuring metal could remarkably augment impact resistance [3], crack
the ability of future generations to meet their own needs [1]. resistance [4], ductility [5], toughness [6, 7] and the tensile
The escalating global population and its ramifications on strength [8–10] of cementitious composites. Nevertheless,
construction industry present notable obstacles [2]. The uti- the manufacturing process of such fibers entails a significant
lization of fiber reinforcement, encompassing metal fibers, consumption of fossil energy, thereby posing a challenge
in striking a balance between performance and cost. The
utilization of natural plant fibers presents a viable solution
Highlights to these challenges owing to their ample availability and
• NaoH-treated pineapple leaf fibers (PALFs) to explore potential
environmentally conscious attributes, such as environmen-
in cementitious composites.
• 6 wt.% NaOH-treated PALF shown highest tensile and young’s tal preservation, biodegradability, and energy efficiency
modulus. [11–16].
• X-ray diffraction (XRD) analysis revealed that NaOH treatment Several endeavors were undertaken to foster organic plant
increased the crystallinity.
fibers within cementitious materials. Fiber treatments are
• Scanning electron microscopy (SEM) analysis showed stable
surface after NaoH treatment. utilized in order to alleviate the significant water absorp-
• Current findings ensure potential of PALF for reinforcement in tion properties exhibited by cellulose fibers. One frequently
structural materials. employed treatment technique for fiber hornification is
implementation of drying and wetting cycles, which result
* Bebitta Robinson Chellathurai
[email protected] in enhanced dimensional stability and more favorable fiber-
matrix interface [17]. According to reference [18], this
1
Department of Civil Engineering, University College particular treatment has the ability to improve structural
of Engineering Nagercoil (A Constituent College of Anna integrity while improving the durability of cementitious
University, Chennai), Konam‑629004, Tamil Nadu, India

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9898 Biomass Conversion and Biorefinery (2024) 14:9897–9913

materials. According to previous research [19], curauá fiber in reduced consumption of chemicals and water [33]. Fur-
has exhibited higher Young’s modulus and tensile strength in thermore, the inclusion of PALF has been found to yield
uniaxial tensile tests when compared to piassava, sisal, coir, substantial enhancements in various mechanical properties,
and jute fibers. Considerable investigation has been under- in comparison to a polypropylene matrix [34]. The impact
taken to examine the fatigue, flexural, physical, fracture, and flexural properties of polyethylene and epoxy compos-
and mechanical characteristics of composites reinforced ites have been improved as a consequence of the addition of
with natural fibers. These studies consistently demonstrate PALF [35]. In a broad sense, cementitious composites that
the advantageous influence of natural plant fibers on flex- incorporate natural plant fibers as reinforcement materials,
ural properties, mechanical, and physical characteristics of such as PALF demonstrate enhanced characteristics in terms
cement-based materials [20–23]. Prior research conducted of impact resistance, ductility, and toughness [35–38]. How-
on utilization of sisal fibers in cement-based composites has ever, there has been relatively less emphasis placed on the
documented the occurrence of a multi-cracking phenomenon examination of cement reinforced with PALF. This study on
characterized by strain-hardening behavior in both bending recently introduced cement PALF indicates the possibility of
and tension as reported [24, 25]. The occurrence of strain- advancing a more resilient and malleable cement composite.
hardening phenomena has also documented in cementitious The research findings on PALF and their effectiveness as
composites containing natural curauá fibers treated with a reinforcement in cementitious composites through NaOH
alkali, as reported in reference [26]. In a separate study, treatment hold significant importance in material science
Bartosz observed strain-softening behavior in alkali-treated and engineering mechanical interlock between the fiber sur-
natural curauá fibers that had undergone weathering due to face and matrix. PALFs’ renewability and ability to enhance
the degradation of bond between the fibers and the matrix mechanical properties make them a promising eco-friendly
[27]. The results of this study indicate the possibility of sub- alternative to synthetic fibers, contributing to sustainable
stituting synthetic and metal fibers with plant-based fibers in construction materials. The study’s insights into PALFs’
cementitious composites. structural changes through XRD and chemical modifica-
Pineapple, being a crop of nonclimacteric ranking as the tions via FTIR offer valuable knowledge for optimizing
third most extensively cultivated plant, produces a substan- fiber-matrix interactions. The research’s significance lies in
tial quantity of crop residue that necessitates appropriate its potential to create durable and corrosion-resistant cemen-
management [28]. Pineapple leaf fiber (PALF) is a notable titious materials, promoting greener construction practices
natural fiber that comes from leaves of plants, distinguished and a resilient built environment.
by its elevated cellulose content and reduced microfibrillar
angle. These characteristics are responsible for the improved
tensile properties exhibited by PALF [29]. The availabil- 2 Materials utilized
ity and impressive mechanical properties of pineapple fiber
have led to its significant recognition in this field. This has The study utilized grade 53 Portland cement, complying
made it a viable option for a wide range of engineering with the specifications of ASTM C 430 [36]. The specific
applications [30]. Nevertheless, the chemical degumming gravity of cement was measured at 3.15, and its chemical
method used in the commercial utilization of pineapple properties is detailed in Table 1. River sand, with a spe-
fiber, including PALF, presents certain obstacles such as cific gravity of 2.57 and a fineness modulus of 2.89, was
environmental contamination and sub-standard fiber char- selected as fine aggregate (Fig. 1a). The sand was properly
acteristics. These challenges render the method detrimental graded and conformed to zone II requirements according
and impede the progress of associated industries [31]. Vari- to ASTM C136 [37]. The bulk density of river sand is
ous methodologies have been investigated by researchers determined to be 1760 kg/m3. Sodium hydroxide (NaOH)
in order to tackle the issue of effectively utilizing PALF. was procured from Astra Chemicals, Chennai, India. The
One example of achieving efficient elimination of impurities research focused on utilizing PALF sourced from the
from PALF involves the utilization of alkaline and silicate Ananas comosus plant, which are locally obtained at a
treatments, which have demonstrated enhanced strength of farmer’s land situated in Kanyakumari, ensuring their
tensile nature [32]. The incorporation of PALF has exhib- availability and freshness. In their natural state, the PALF
ited encouraging outcomes, as it has effectively decreased measured approximately 15–20 cm in length, offering
the amount of residual gum present and has also resulted ample material for study. The PALF derived from these

Table 1  Chemical properties of Components SiO2 Fe2O3 SO3 Al2O3 MgO3 CaO Na2O K2O IR Cl LOI
cement
Cement 22.1 3.7 2.7 3.2 1.3 64.2 0.3 0.12 0.3 0.02 1.9
Biomass Conversion and Biorefinery (2024) 14:9897–9913 9899

into 2-cm lengths and subjected to thorough testing prior

to their incorporation of testing.

2.1 About pineapple leaf fiber

The annual production of PALF generates a significant quan-

tity of fibrous material, with only a small portion currently
utilized in feedstock and utility production [38]. The increas-
ing popularity of biocomposites has created opportunities
for broader industrial applications, reducing waste of renew-
able resources and fostering on composites and engineering
sector [39]. PALF possesses notable strength and stiffness
properties [40–42]. The extraction of fibers from pineap-
ple leaves involves mechanical extraction and retting meth-
ods. Studies have shown that approximately 2–3% of fibers
can be extracted from fresh leaves [43]. Also, the PALF’s
fibrous cellulosic structure, consisting of vascular bundles
organized in clusters, offers excellent bonding capabilities
when incorporated into cementitious matrices for retrofit-
ting application to increase the durability and mechanical
properties of concrete elements such as beams, columns,
and slabs. PALF’s chemical composition, including poly-
saccharides, lignin, and other constituents, contributes to
its compatibility with composite matrices and its ability to
improve the overall performance in its utilization [44]. The
fibers themselves are composed of closely interconnected
slender multicellular fiber cells held together by pectin [45].
Cellulose constitutes a substantial portion of PALF rang-
ing from 70 to 82%, exhibiting a fiber arrangement similar
to that of cotton (82.7%), where the strength and stiffness
depend on the cellulose forming the rigid network with mor-
Fig. 1  a Particle size analysis of fine aggregate. b Extracted PALF tar [46, 47]. PALF has demonstrated enhanced mechanical
strength compared to jute fibers when used in the production
of fine yarn, as supported by sources [48]. PALF represents
Table 2  Physical properties of PALF a significant natural fiber resource with excellent compat-
Physical properties Percentage
ibility and a favorable chemical composition. Its remarkable
properties including torsional rigidity, flexural properties,
Cellulose (%) 71–83 rigidity, and high specific strength make it a viable alterna-
Lignin (%) 5.2–13.7 tive raw material for reinforcing material composites [49].
Pectin (%) 1.3
Hemicellulose (%) 17.6 2.2 Pineapple leaf fiber extraction
Density (g/cm3) 0.92
Microfibrillar angle (deg) 15 The extraction and treatment of PALF involve a systematic
Moisture content (%) 12.6 and carefully controlled process aimed at obtaining high-
Diameter (µm) 20–80 quality fibers for various applications. The procedure begins
with retting, soaking, and mechanical separation of fibers
from the leaves, as shown in Fig. 2. This technique involves
leaves exhibited desirable characteristics, including an the careful removal of leaves to extract the elongated and
aspect ratio of 100, a distinctive dark green coloration, and slender fibers embedded within. To facilitate fiber extrac-
a Young’s modulus of 1.44 GPa. The properties of PALF tion, mature harvested pineapple leaves undergo a prolonged
are given in Table 2, and these attributes make PALF a soaking period of 4 weeks in water, softening the leaves
promising reinforcement material for cementitious com- and facilitating easier fiber isolation. During this soaking
posites. These leaves were carefully manually chopped process, microbes, such as bacteria and fungi, enzymatically
9900 Biomass Conversion and Biorefinery (2024) 14:9897–9913

Fig. 2  a Discarded pineap-

ple leaf. b Retting process.
c Soaked in urea solution. d
Removal of fiber. e Extracted
PALF

break down the hemicellulose present in the leaves, enhanc- conducted for each of the above treatment conditions, allow-
ing the release and isolation of fiber bundles. Subsequently, ing for comprehensive analysis and evaluation of the effects
a thorough washing procedure is employed using deionized of different alkali solution concentrations on the properties
water to eliminate residues and impurities that may be pre- of PALF samples.
sent on fiber surface, ensuring durability and longevity of
fibers. After washing stage, the fibers undergo controlled 2.3 Tensile test of PALF
drying for 15 days at a temperature of 26 °C, effectively
removing excess moisture and preparing them for further Tensile experiments were performed on samples of PALF both
treatment and characterization. PALF samples are treated in untreated and treated state with NaOH at varying concentra-
with various levels of NaOH solutions to study the effects tions of 2 wt.%, 4 wt.%, 6 wt.%, and 8 wt.% in accordance with
of alkali treatment. Alkali solutions with concentrations of the prescribed protocols described in ASTM C1557-14 [50].
2 wt.%, 4 wt.%, 6 wt.%, and 8 wt.% are prepared, and the The experiments were conducted utilizing servo controlled
fiber samples are soaked in respective solutions for 1 h at Lawrance and Mayo Force Test Stand, which was outfitted
26 °C. Subsequent rinsing with deionized water is carried with a capacity of load 1.5 kN. In order to mitigate the occur-
out until reaching a neutral pH of 7, removing any residual rence of fiber slippage from the grip, the fiber specimens are
alkali solution or impurities. The rinsed fibers are then air- affixed and properly fixed on wood sheet utilizing adhesive
dried at 26 °C for 24 h to complete the treatment process. cyanoacrylate, thereby establishing robust mounting tab. Ten-
To ensure accurate characterization, parallel experiments are sile tests were done with a steady crosshead shift at a pace of
Biomass Conversion and Biorefinery (2024) 14:9897–9913 9901

18 mm/min in a temperature of 25 °C and 76% relative humid- initial cross-sectional area into account, the mean force at
ity. The experimental setup involved setting the gauge length which every specimen shattered, was utilized to compute the
at 25 mm and conducting a minimum of three replicates for corresponding tensile strength using Eq. (2). As a result, the
each sample to ensure reliability and accuracy of results. The conducted tensile tests yielded significant findings regard-
force–displacement data was obtained directly using comput- ing the mechanical characteristics of the PALF samples,
erized testing to determine the tensile properties. The examina- facilitating the evaluation of their tensile strength as shown
tion of NaOH-treated PALF samples unveiled discrepancies in in Fig. 3a. The assessment of the tensile properties plays a
fiber diameter. To determine the diameter of fiber, the broken crucial role in determining the appropriateness of PALF for
end located within the defined length of gauge is measured uti- different applications and contributes to a comprehensive
lizing a micrometer screw gauge. The fragmented fiber distinc- comprehension of its performance.
tive cross-sectional dimension was calculated using equation:
2.4 SEM, XRD, and FTIR analysis of PALF
A = 𝜋d2∕4 (1)
In the given context, A—symbolizes the fibers area cross Scanning electron microscopy (SEM) analysis is conducted
section, while d represents the diameter of fiber. The ini- on PALF samples to investigate their surface morphology
tial cross-sectional area of fragmented fiber is subsequently and microstructural features. The samples were prepared
employed to ascertain tensile strength of fiber that was by mounting small sections onto SEM stubs and sputter-
subjected to testing. The calculation of tensile strength (s) coating them with a thin layer of conductive material. The
involved dividing the force experienced by fiber at the point SEM images revealed the fibrous nature of PALF showing
of fracture (F) by the initial cross-sectional area (A) of fiber their elongated and slender structures and provided insights
at that same point. This relationship is represented by the fol- into fiber’s texture. Moreover, the high-resolution images
lowing equation: captured fine details such as surface irregularities, fiber
diameter variations, and the presence of any contaminants or
𝜎 = F∕A (2) impurities. SEM analysis helps in characterizing the physical
properties and surface characteristics of PALF enhancing the
Equation (2) represents the relationship between the ten-
structural knowledge and application potential.
sile strength (s) of a material and applied force (F) divided
X-ray diffraction (XRD) spectra of sample powder have
by the cross-sectional area (A) of material. Taking Eq. (1)’s
been collected via Malvern diffractometer that comes with

Fig. 3  a Tensile testing of PALF. b Compression test on PALF composite cubes. c Flexural test on PALF composite prism
9902 Biomass Conversion and Biorefinery (2024) 14:9897–9913

(λ = 1.54060 Å) CuKα monotonous radiation. The equip- mixture with and without fiber treatment was determined
ment worked with an applied voltage of 45 (kV) kilovolts using the penetration resistance method with cubed molds
having 40 (mA) milliamperes current. T scattering intensi- following the standard technique [56]. Followed curing in
ties were scanned from 5 to 45° at a resolution of 0.05°. To the ambient environment for 28 days at 23 °C, six prismatic
determine the degree of crystallinity in untreated and treated specimens of each combination were subjected to mechani-
PALF samples, according to Segal [51], empirical technique cal testing in their solid form. The evaluation of mechanical
was based on the height of peaks to determine the crystallin- strength involved compressive and flexural tests (Fig. 3b and
ity percentage. The calculation of the percentage crystallin- c) using a universal testing machine, following the specifica-
ity (C) was performed using the following equation: tions outlined by ASTM [32, 33]. Durability-related factors
were also investigated through tests measuring water absorp-
C = (I002 ∕IAM ) × 100% (3) tion by capillary pores. Water absorption by capillary pores
The variable I002 denotes the peak intensity associated analyzed the intercommunication of internal pores, while
with highest crystalline peak intensity. The amplitude of the immersion in water examined the apparent pores and their
diffraction pattern in non-crystalline material is represented volumes. These tests provided insights into the durability of
by IAM, commonly referred to as the amorphous band. The mortar mixtures. The capillary water absorption test involved
depression between the crystalline peaks is a measure of vertically positioning the specimens on a 20-mm constant
its intensity. The Debye–Scherrer relation (D) was used to water slide, and the mass of water bodies was measured after
estimate sample crystallite sizes. The equation for D can be 90 min of exposure. The mortars compressive strength was
expressed as follows: measured using 70.6-mm, 70.6-cm cube specimens after
curing for 28 days. The tests were performed using an MTS
D = K𝜆∕(b × cos𝜃) (4) testing machine with a 2000-kN capacity and a deformation
velocity of 0.1 mm/min, in accordance with ASTM C109
In the given context, the crystallite size denotes D, the
at a laboratory. A three-point bending test was conducted
wavelength of CuKα radiation is denoted by λ, b corresponds
on prism with dimensions of 160 mm × 40 mm × 40 mm in
to the fraction angles at which the full-width at half-maxi-
order to measure the flexural strength of mortar. The evalu-
mum (FWHM) is measured, K denotes the factor of correc-
ation was carried out with the assistance of a universal test-
tion 0.86, and the term θ signifies the highest peak diffrac-
ing machine that has a capacity of 1000 kN and a speed of
tion angle observed in the PALF samples.
0.1 mm/min. Also, the distance of 120 mm was determined
In Fourier-transform infrared (FTIR) analysis, the treated
to be the span between the supports.
and untreated PALF samples were fragmented into small
particles measuring approximately 1 mm in size. The sam-
ples were subsequently subjected to analysis using a Bruker
3 Results and discussions
Nano-NanoIR spectrometers, manufactured by Bruker
Co. Ltd. The spectrometer was equipped with an attenu-
3.1 Tensile studies of PALF
ated total reflectance (ATR) attachment. The FTIR spec-
tra were obtained within the wavenumber interval of 500
The tensile testing of PALF samples revealed distinctive
to 4000 ­cm−1 utilizing a spectral resolution of 4 ­cm−1 and
young’s modulus (Fig. 4a) and tensile strength (Fig. 4b)
16 scans. The objective of this analysis was to ascertain the
for untreated and differentially treated specimens. The
functional groups that were present in PALF samples both
mechanical properties, including strain at break, Young’s
prior to and after treatments.
modulus, and ultimate tensile strength (UTS) are summa-
rized in Table 3. It is evident that treatment with NaOH
2.5 Mix proportions and mechanical testing of PALF at various concentrations had a significant impact on
mortar mechanical properties of PALF. The treated PALFs exhib-
ited lower strains at break, with values showing a percent-
The mortar was prepared using a mass ratio of 1:3 age decrease compared to untreated PALF. Specifically,
(cement:sand) as commonly used in the literature for struc- the strains at break for treated PALFs (2 wt.%, 4 wt.%,
tural repair mortars [52]. Fibers were incorporated at pro- 6 wt.%, and 8 wt.% NaOH) decreased by approximately
portions of 0% (reference), 0.5%,1%,1.5%, 2%, 2.5%, and 6.3%, 5.1%, 7.6%, and 7.6% respectively, in comparison to
3% by mass of cement. The fluidity of mortar was assessed untreated PALF 8.9%. Moreover, the treated PALFs dem-
using a standard slump table test according to ASTM stand- onstrated substantially higher UTS values, with a percent-
ards [53]. Technological tests were conducted in fresh state age increase in UTS compared to untreated PALF. The
to measure setting time, drying shrinkage, water absorp- UTM values for treated PALFs (2 wt.%, 4 wt.%, 6 wt.%,
tion, and sorptivity tests [54, 55]. The setting time of each and 8 wt.% NaOH) increased by approximately 147.7%,
Biomass Conversion and Biorefinery (2024) 14:9897–9913 9903

Fig. 4  a Young’s modulus of

PALF. b Tensile strength of
PALF

Table 3  Mechanical properties of PALF with an impressive percentage increase of approximately

S. No Specimen Strain at Young’s Ultimate tensile
157.2% compared to untreated PALF. These changes in
break (%) modulus strength (MPa) fiber stress and strain values indicate an increase in stiff-
(GPa) ness and a decrease in strain at break for treated PALFs,
making them potentially suitable as reinforcement materi-
PF0 Untreated 8.9 11 788
als for various composite applications. Furthermore, the
PF2 NaOH 2% 5.1 29 1363
treated PALFs exhibited higher Young’s modulus values,
PF4 NaOH 4% 6.3 35 1950
with percentage increases in Young’s modulus for treated
PF6 NaOH 6% 7.6 32 2025
samples (2 wt.%, 4 wt.%, 6 wt.%, and 8 wt.% NaOH) com-
PF8 NaOH 8% 7.6 20 1375
pared to untreated PALF. The Young’s modulus values
for treated PALFs increased by approximately 218.2%,
163.6%, 190.9%, and 81.82% respectively, showcasing the
72.97%, 156.98%, and 74.49% respectively compared to enhanced rigidity and stiffness achieved through NaOH
UTS of untreated PALF. Among the treated PALFs, the treatment. These findings highlight the effectiveness of
sample treated with 6 wt.% NaOH exhibited highest UTS, NaOH treatment in modifying the mechanical properties
9904 Biomass Conversion and Biorefinery (2024) 14:9897–9913

of PALF, making it a promising candidate for enhancing Table 4  Crystallinity properties of raw and treated PALF composites
the performance of composite materials. Specimen Crystallite size (nm) Crystallinity (%)

3.2 XRD studies of PALF composites Untreated 20.01 65.31

NaOH 2% 21.60 69.20
The XRD patterns of both treated and untreated pineapple NaOH 4% 23.10 70.77
leaf fibers (PALFs) composites are depicted in Fig. 5. The NaOH 6% 25.92 79.38
results obtained demonstrate a consistent cellulose I crys- NaOH 8% 24.98 75.18
tal pattern, characterized by a prominent peak at 2θ posi-
tion of 22°, which corresponds to the reflection of (002)
plane. Furthermore, it is worth noting that a slight increase offers significant insights into the structural characteristics
in intensity is observed at a 2θ angle of 15.1°, which can of processed PALF. The alterations in crystallinity and crys-
be attributed to reflection of (101) plane in both untreated tallite size observed indicate that application of NaOH treat-
and treated PALFs [57]. Nevertheless, it has been observed ment affects the internal structure of PALF, thereby influenc-
that treated PALF with a sodium hydroxide concentration ing its properties. The aforementioned discoveries enhance
of 8 wt.% exhibits a distinct peak split at (101) plane reflec- our comprehension on impact of NaOH treatment on crystal-
tion at 2θ positions of 15.0° and 16.6° [58]. Table 4 illus- line characteristics of PALF, thereby playing a crucial role
trates the mean values of crystallite size and crystallinity in customizing their properties to suit diverse applications.
for both treated and untreated PALF composites. The find-
ings indicate that crystallinity of PALFs subjected to NaOH 3.3 FTIR studies of PALF composites
treatment ranging from 2 to 8 wt.% exhibited an increase in
comparison to untreated PALF. However, it is noteworthy The FTIR spectra of untreated and treated PALF compos-
that treated PALF with a NaOH concentration of 8 wt.% ites are depicted in Fig. 6, covering the wavenumber range
demonstrated a decrease in crystallinity. The treated PALF of 500–4000 ­cm−1, the display of spectra distinct bands of
samples with varying NaOH concentrations displayed a zig- absorption at approximately 1028, 1112, 1171, 1435, 1629,
zag pattern in terms of crystallite size. The observed trend 2921, and 3347 ­cm−1. Cellulose, the primary component
is an increase in measured parameter from untreated PALF of PALF, has a spectral peak at 3347 ­cm−1 indicating the
to PALF treated with 2 wt.% NaOH. Subsequently, there is presence of O–H group functionals. The bands of transmis-
a decrease in measured parameter for the PALF treated with sion observed at 2921 ­cm−1 and 1629 ­cm−1 were identified
4 wt.% NaOH. However, the measured parameter increases as stretching of C–H bond and presence of water absorbed
again for the PALF treated with 6 wt.% NaOH. Finally, there respectively [59]. The spectral peak observed at a wave-
is another decrease in measured parameter for PALF treated number of 1435 ­cm−1 can be attributed to bending motion
with 8 wt.% NaOH. The X-ray diffraction (XRD) analysis of O–H bond. Additionally, the spectral peaks observed at
wavenumbers of 1171 ­cm−1, 1112 ­cm−1, and 1028 ­cm−1 are

Fig. 5  XRD analysis of untreated and treated PALF composites Fig. 6  FTIR analysis of treated and untreated PALF composites
Biomass Conversion and Biorefinery (2024) 14:9897–9913 9905

indicative of stretching motion of C–O–C bond in β-1,4- [63]. The cementitious substrate was expected to absorb
glycosidic linkage [58]. When examining the untreated energy better with smooth natural plant fibers. It is note-
and treated PALFs, two noteworthy observations can be worthy that the surface shape did not alter noticeably after
discerned. To begin with, the PALF spectrum that has not being immersed in NaOH solutions [64–66]. This indi-
undergone any treatment (Fig. 6) displays a solitary promi- cates the durability of fiber surface under these conditions.
nent peak at around 1253 ­cm−1, which can be attributed to In addition to aspect ratio and fiber length, studies have
C–O lignin stretching. However, in the spectra subsequent emphasized the significance of bonding behavior between
spectrum above (Fig. 6), the aforementioned band becomes cement matrix and fibers in determining the composites
undetectable, while two distinct bands emerge at approxi- properties, particularly in terms of flexural toughness [35].
mately 1247 ­cm−1 and 1215 ­cm−1 were identified as C–OH Understanding and optimizing this bond behavior are cru-
bending [60]. Furthermore, the observed decrease in inten- cial for enhancing the overall performance of fiber-rein-
sity of prominent and distinct peak near 1726 ­cm−1 was due forced cementitious composites. The findings presented
to the presence of carbonyl and ester (C = O) functional in this section demonstrate that surface morphology of
groups in hemicellulose and lignin, directly correlated with PALF remains relatively stable even after exposure to
increase in NaOH concentration being involved in bond- NaOH solutions.
ing in which the respective groups will disappear. Never-
theless, the spectral analysis of PALF subjected to 8 wt.%
NaOH treatment reveals the persistence of band located at 3.5 Physical properties of fresh and hardened PALF
1726 ­cm−1. The aforementioned observations suggest that composites
there are reactions taking place between the lignocellulosic
fiber and NaOH [61]. The FTIR analysis offers significant The evaluation of physical characteristics of hardened and
insights in the chemical transformations occurring in poly- fresh mortars was performed by means of water absorption,
meric aromatic lignin fractions (PALFs) following treatment drying shrinkage, setting time, and sorptivity. Table 5 dis-
with sodium hydroxide (NaOH). The absence of lignin- plays the mean setting durations of mortar mixtures. Gener-
related spectral band and observed changes in the intensi- ally, the setting times appeared to be prolonged with increas-
ties of bands associated with functional groups suggest that ing PALF content. However, when 2.5 wt.% PALF was
fiber structure has been effectively modified making their included, there is a decrease in setting time. This could be
prospective applications across diverse domains. attributed to excess fibers absorbing water, causing the mix
to set more quickly. The drying shrinkage behavior of mortar
3.4 Microstructural studies of PALF composites mixes was evaluated as shown in Fig. 8. Each mix containing
different ratios of PALF exhibited distinct shrinkage behav-
Natural plant fiber resilience in composites made of ior. The rate of shrinkage increase was high for all mortars,
cement is a significant area of concern [15]. Cement, as a except for mixture with 0 wt.% PALF, which can be attrib-
strongly alkaline material, yields a substantial quantity of uted to curing process. After 28 days, it can be observed that
calcium hydroxide during hydration process, which can inclusion of PALF helped in reduced shrinkage. Notably, the
impact the performance of natural plant fibers [62]. In this mortar mixes reinforced with 2.5 wt.% PALF exhibited least
study, we will examine how NaOH affects the morphology shrinkage. This finding aligns with the results reported by
of fiber surface and the tensile strength of cementitious Singh et al., who demonstrated that a higher volume fraction
composites made with natural plant fibers. Scanning elec- of oil palm trunk fiber (4 wt.%) reduced shrinkage for vari-
tron microscopy with a CIQTEK SEM 5000 was utilized ous core diameters [67]. The sorptivity and water absorption
to evaluate the morphological surface of natural plant fib- test results for mortar mixes are depicted in Fig. 9a and b
ers, as illustrated in Fig. 7. Both treated and untreated respectively. The mortar reinforced with 3 wt.% amount of
PALF with NaOH solution for 28 days are subjected to PALF demonstrated the greatest capacity for water absorp-
drying at 100 °C and subsequently coated with a layer of tion rate, whereas the reference sample displayed least
gold before analysis. Figure 7 shows that monofilament capacity of water absorption rate which is similar to other
fibers had irregular features, including lateral branches and findings [68, 69]. The mortar mixes containing 1 to 2 wt.%
center cavities. The degumming procedure eliminated sur- PALF exhibited a reduction in both water absorption rate
face contaminants, resulting in fibers with an impeccable when compared to mixes containing 2.5 wt.% and 3 wt.%
surface. It was found that the interaction of chemicals and PALF. While there may be variations in findings compared
interfacial interaction among the cementitious matrix and to certain published studies, the results presented in this
fibers might be decreased due to smooth surface. Thus, study align with other research and indicate that utilization
instead of fiber breakage, the specimens showed pullout of natural fibers, such as palm fibers, enhances the capacity
behavior, which resulted in greater energy absorption for water absorption and sorptivity [70–72].
9906 Biomass Conversion and Biorefinery (2024) 14:9897–9913

Fig. 7  SEM image of PALF

composite. a Untreated. b 2%
NaOH treated. c 4% NaOH
treated. d 6% NaOH treated. e
8% NaOH treated

Table 5  PALF mortar setting time 3.6 Compressive strength of PALF composites

Mix no Fiber inclusion (wt.%) Average setting time
(hrs)
The compressive strength of PALF mortar was evalu-
ated at different curing ages, and the results are displayed
Initial Final in Fig. 10. At 7 days of curing (Fig. 10a), the mortar
PF0 0 03:00 04:00 without PALF (PF0) exhibited a compressive strength
PF0.5 0.5 03:15 04:20 of 9.26 MPa, which served as reference point for com-
PF1 1 03:30 04:15 parison. With the addition of 0.5 wt.% PALF (PF0.5),
PF1.5 1.5 04:25 05:15 the compressive strength increased to 10.20 MPa, repre-
PF2 2 04:05 04:50 senting a 10.15% increment. This trend continued with
PF2.5 2.5 03:15 03:50 higher fiber content, showing significant improvements
PF3 3 02:25 03:05 in compressive strength. At 28 days of curing (Fig. 10b),
Biomass Conversion and Biorefinery (2024) 14:9897–9913 9907

positioning them as a promising contender for reinforcing

cementitious composites.

3.7 Flexural strength of PALF mortar

The flexural strength of PALF mortar was evaluated at both

7 days and 28 days, and the results are presented in Fig. 11a
and b respectively. It is evident that the incorporation of
PALF had a significant impact on the flexural strength of
mortar. At 7 days, the flexural strength increased progres-
sively with the addition of PALF. The mortar containing
2.5 wt.% PALF displayed the highest flexural strength of
4.41 MPa, representing a substantial 54.74% increment
compared to fiber-free mortar (PF0) with a flexural strength
of 2.85 MPa at 7 days. Similarly, at 28 days, the trend con-
tinued, and the mortar with 2.5 wt.% fibers exhibited the
highest flexural strength of 5.07 MPa, reflecting a remark-
Fig. 8  Drying shrinkage of PALF composite
able 48.25% increment over PF0 with a flexural strength
of 3.42 MPa as shown in Fig. 11; beyond 2.5 wt.% fiber
content, there is a slight decrease in flexural strength trend
similar trends were observed. The reference mortar (PF0) which is 32.60% at 3 wt.% fiber content. The reinforcement
showed a compressive strength of 17.5 MPa, while the effect on mortar is evident, leading to enhanced flexural
inclusion of 0.5 wt.% PALF (PF0.5) resulted in a compres- strength. Additionally, the incremental percentage improve-
sive strength of 20.50 MPa, representing a 17.14% incre- ments achieved by PALF at both 7 days and 28 days are
ment. As the PALF content increased to 1 wt.%, 1.5 wt.%, competitive compared to other natural fibers. These results
2 wt.%, and 2.5 wt.%, the compressive strength continued highlight the potential of PALF as an eco-friendly and effec-
to rise significantly with increments of 21.14 wt.%, 30.29 tive alternative for enhancing the flexural strength of cemen-
wt.%, 33.43 wt.%, and 39.43 wt.% respectively; beyond titious composites. Moreover, their wide availability and
2.5 wt.% fiber content, there is a slight decrease in com- sustainable sourcing make them an attractive option for use
pressive strength trend which is 24.86% at 3 wt.% fiber in construction materials, contributing to the development
content. These findings indicate that addition of PALF to of greener and more durable infrastructure. The observed
the mortar significantly enhances its compressive strength enhancement in mechanical strength for 2.5 wt.% fiber com-
at fiber contents upto 2.5 wt.%. Comparing this to other position can be attributed to treatment-induced increase in
fiber-reinforced mortars, PALF has demonstrated excellent specific surface area of fibers. This increase enables the
potential as a reinforcement material. Its ability to improve PALF to serve as transfer points for applied forces, result-
the compressive strength of mortar suggests that it can be ing in improved ductility and resistance of mortar [15]. The
a viable and cost-effective alternative to traditional fibers observed decline in strength at 3 wt.% fiber mixes can be
used in construction applications. Furthermore, the stable attributed to the saturation of fibers within the cementitious
and durable characteristics of PALF as observed in this matrix. It is widely recognized that composites which exhibit
study, make it a promising candidate for further explo- an optimal fiber content maximizes the material strength.
ration in various construction and composite materials. When the percentage of fiber incorporation exceeds this
Prior research has demonstrated that the incorporation maximum content, the fibers tend to agglomerate within the
of NaOH-treated fibers in mortars resulted in a notable matrix due to inadequate wettability as documented in previ-
improvement in flexural strength [73–75]. Likewise, the ous studies [76–78].
compressive strength properties demonstrated a compara-
ble trend. The inclusion of 2.5 wt.% treated PALF resulted 3.8 Rapid chloride penetration test of PALF mortar
in a notable enhancement in compressive strength. The
results of this study demonstrate the positive impact of The rapid chloride test conducted on PALF mortar speci-
NaOH treatment on mechanical characteristics of PALF, mens provided valuable insights into their ability to resist
indicating their capacity to improve the overall durabil- chloride ion penetration, a crucial factor in assessing the
ity of mortar. The utilization of an optimal proportion of durability of cementitious materials. The results presented
treated PALF has potential to yield significant enhance- in Fig. 12 clearly demonstrate the positive impact of PALF
ments in both flexural and compressive strength, thereby on reducing chloride ion ingress in the mortar. Notably,
9908 Biomass Conversion and Biorefinery (2024) 14:9897–9913

Fig. 9  a Sorptivity of PALF.

b Water absorption of PALF
composite

specimens with higher percentages of PALF (PF1, PF1.5, making them effective inhibitors against chloride ingress
PF2, and PF2.5) exhibited the most remarkable perfor- [80]. The observed increase in chloride diffusion coefficient
mance, showing a “Very Low” level of chloride ion pen- with increasing PALF content as shown in Fig. 12 suggests
etration. This indicates that PALF effectively act as barriers, that the incorporation of PALf affects the molecular filter-
preventing the infiltration of chloride ions into mortar and ing process within nanopores, leading to enhanced chloride
thereby enhancing its resistance to chloride-induced cor- resistance. The deeper penetration of chloride ions in the
rosion. Even at lower fiber percentages (PN0.5 and PN3), plain control compared to PALF-reinforced composites
the chloride ion penetration remained at the “Low” level, further underscores the protective effects of PALF. In con-
indicating that even a small amount of fiber reinforcement clusion, the rapid chloride test results strongly support the
can confer notable benefits in terms of chloride resistance. use of PALF in cementitious composites to improve their
Comparing the findings with other fiber-reinforced mortars, durability and longevity, especially in harsh environments
PALF stands out for their promising performance in miti- with chloride exposure. Their unique properties and poten-
gating chloride ion penetration [79]. Their unique surface tial molecular filtering capabilities make them a valuable
characteristics and the potential formation of a protective and eco-friendly option for enhancing the performance of
layer around the fibers hinder the movement of chloride ions, construction materials.
Biomass Conversion and Biorefinery (2024) 14:9897–9913 9909

Fig. 10  Compressive strength

of PALF composite. a 7 days. b
28 days

4 Conclusions tensile strength (UTS) and Young’s modulus compared to

untreated PALF. PALF treated with 6 wt.% NaOH dem-
PALFs treated with various concentrations of sodium onstrated better properties showcasing the effectiveness
hydroxide (NaOH) to investigate their potential as rein- of NaOH treatment with enhanced stiffness and strength.
forcement materials for cementitious composites in XRD analysis showed NaOH treatment increased the crys-
structural and building applications. The mechanical tallinity of PALF, except for sample with 8 wt.% NaOH,
properties, crystalline characteristics, and microstruc- which exhibited a decrease in crystallinity. The crystallite
ture of treated PALFs were analyzed, and their effects size of PALFs varied with NaOH concentration, indicating
on physico-mechanical properties of mortar mixes were structural modifications due to treatment. FTIR analysis
evaluated. Tensile test revealed treated PALFs exhibited revealed chemical transformations in PALF structure fol-
lower strains at break but substantially higher ultimate lowed by NaOH treatment. The absence of lignin-related
9910 Biomass Conversion and Biorefinery (2024) 14:9897–9913

Fig. 11  Flexural strength of

PALF composite. a 7 days. b
28 days

bands and changes in intensities of functional group bands shrinkage as well as the water absorption and sorptivity
indicated effective modification of the fiber structure. increased with higher fiber content, but mortar mixes with
SEM analysis showed surface morphology of PALFs 1 to 2 wt.% PALF showed lower absorption rates. Incor-
remained stable after NaOH treatment, indicating their poration of PALF significantly enhanced both compressive
potential as reinforcement materials in cementitious com- and flexural strengths of mortar. The mortar with 2.5 wt.%
posites. Also, the addition of PALF to mortar influenced PALF exhibited highest compressive and flexural strengths,
its physical properties; the setting time was prolonged with indicating their potential as effective reinforcement materi-
increasing fiber content, but 2.5 wt.% PALF reduced the als in cementitious composites; the volume of permeability
setting time. In addition, the 2.5 wt.% PALF exhibited least decreases, and the transfer of stress will be enriched. Also,
Biomass Conversion and Biorefinery (2024) 14:9897–9913 9911

Fig. 12  Chloride ion penetra-

tion test of PALF composite

the PALF acted as barriers, reducing chloride ion penetra- Consent for publication Written formal consent ensures that the pub-
tion in mortar. Higher fiber contents (PF1.5, PF2, PF2.5, lisher has the author’s permission to publish research findings.
and PF3) showed most significant reduction in chloride ion Competing interests The authors declare no competing interests.
penetration, indicating their efficacy in enhancing the mor-
tar’s resistance to chloride-induced corrosion.
To conclude, the NaOH-treated PALF exhibited improved
mechanical properties, crystalline characteristics, and micro-
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