Enhancing Jute Fiber Properties with TiO2
Enhancing Jute Fiber Properties with TiO2
REGULAR ARTICLE
Abstract
This study introduces a novel, synergistic surface modification approach combining peracetic acid (PAA) treatment, TiO2
nanoparticle coating, and gamma irradiation to significantly enhance jute fibers' mechanical strength, surface morphology,
crystallinity, and water resistance. Integrating these three unique methods enables profound structural alteration and surface
functionalization, resulting in a more hydrophobic, durable, and mechanically robust fiber. The strategic sequence of treat-
ments promotes adequate T iO2 adhesion, fiber densification, and improved fiber matrix compatibility. This approach addresses
critical limitations in raw jute fiber performance and offers a scalable path forward for bio-based composite development in
packaging, textiles, and other industrial applications. Raw jute fibers exhibited low breaking force and high water absorp-
tion. TiO2 coating improved these properties, with further enhancements observed upon gamma irradiation at 3 kGy. The
most significant improvements were the chemical treatment to remove lignin and hemicellulose (cellulose JF) and per-acetic
acid (PAA) treatment, combined with TiO2 coating and gamma irradiation. PAA-treated fibers showed the highest breaking
force (492.23 N, a 112% increase compared to raw fibers), tensile strength (169.85% increase), elastic modulus (237.26%
increase), and toughness (116% increase). These fibers also exhibited the lowest moisture content (3.86%, a 67.54% reduc-
tion), moisture regain (4.01%, a 70.24% reduction), and water absorption (102.26%, a 52.92% reduction), along with the
highest water contact angle (86.25°, a 117.51% increase). SEM analysis revealed that PAA treatment resulted in a more
compact and uniform fiber structure, promoting better TiO2 adhesion and mitigating some micro-cracking induced by gamma
radiation. FTIR spectroscopy confirmed the presence of T iO2 and indicated significant structural changes, especially with
PAA treatment. Crystallinity also increased with each treatment step, reaching a maximum of 83.53% for the PAA-treated
fibers. These findings demonstrate the synergistic effects of T iO2 coating, gamma irradiation, and chemical treatments in
enhancing the properties of jute fibers for high-performance applications.
Keywords Mechanical · Physio-chemical · Water resistance · TiO2-coated jute fibers · Gamma irradiation · Chemical
treatments · Crystalinity
4
* Nayem Hossain Department of Chemical Engineering, Dhaka University
[Link]@[Link] of Engineering and Technology (DUET), Gazipur 1707,
Bangladesh
1
Department of Mechanical Engineering, Dhaka University 5
NARP Research Lab, IUBAT-International University
of Engineering and Technology (DUET), Gazipur 1707,
of Business Agriculture and Technology, Dhaka 1230,
Bangladesh
Bangladesh
2
Department of Materials and Metallurgical Engineering, 6
Institute of Radiation and Polymer Technology, Atomic
Dhaka University of Engineering and Technology (DUET),
Energy Research and Establishment, Baipayl, Bangladesh
Gazipur 1707, Bangladesh
3
Department of Mechanical Engineering,
IUBAT-International University of Business Agriculture
and Technology, Dhaka 1230, Bangladesh
Vol.:(0123456789)
Fibers and Polymers
modify fibers, chemical treatment techniques frequently Dhaka-1217, while sodium hydroxide and chlorite were pro-
use reagent functional groups that react effectively with cured from Merck, Ger many. For each investigation step,
the fiber's structure and can eliminate non-cellulosic deionized water was acquired from PureTech, Dhaka-1203,
impurities. This surface modification technique improves Bangladesh. Titanium Isopropoxide (TTIP) and polyvinyl
interfacial adhesion by improving the link between fibers alcohol (PVA) were collected from Sisco Research Laborites
and the polymer matrix in composite materials [22, 23]. Pvt. Ltd., India.
Peracetic acid (PAA) increases the fibers' surface energy,
which promotes TiO2 nanoparticles' uniform distribution 2.2 Chemical Treatment Process
and robust adherence [24]. The limitations of jute fibers
can be creatively addressed by combining T iO2 coating The NaOH solution used for alkali treatment of jute fibers
with gamma irradiation and chemical treatments [25]. has a concentration of 1%. Temperature and time of 30 min
Although a single T iO2 NP might not be able to satisfy and 30 °C are utilized in this experiment. In general, ele-
every need, customizing and doping engineering—par- vated temperatures and times hasten the process but may
ticularly "gamma rays (γ) irradiation" offer viable ways also heighten the danger of fiber injury [5, 10]. This experi-
to enhance TiO 2NPs' capabilities as photocatalysts for ment utilizes oxidative modification with 0.7% NaClO2, with
Hydrogen Evolution Reduction (HER). By improving the a time and temperature of 80 min and 80 °C, as a chemical
physicochemical properties of T iO2NPs, gamma rays can treatment approach to modify the chemical composition of
increase their photocatalytic activity [31]. Scholars have the fibers, resulting in modifications to their properties, such
examined the combined impacts of chemical treatments, as those found in cellulose jute fibers [31]. An acid hydroly-
gamma irradiation, and titanium dioxide ( TiO2) coatings sis process will eliminate the amorphous region where per-
as a comprehensive approach to improving the functional acetic acid is used, producing a highly crystalline substance
properties of jute fibers [16, 19, 26]. known as microcrystalline cellulose [32]. However, it is
The researchers are also working to develop versatile tex- essential to maintain a chemical concentration of 1.5 moral-
tiles using MXenes, plasma activation, silkworm silk, etc. ity, 50 °C temperature, and time 120 min for this process.
[27–29]. Fabrics are also being used to create artificial bone An investigation was carried out to determine the struc-
[30]. tural changes resulting from PAA's removal of non-cellu-
This study examines how gamma irradiation and crystal- losic materials from jute fibers [33].
linity modification work together to improve the mechani-
cal, physio-chemical, and water resistance qualities of T iO2 2.3 Gamma Irradiation
coated jute fibers. Four different kinds of samples were
created to assess the effects of T iO2 coating, gamma irra- XRD data requires several steps to determine crystallinity;
diation, and chemical treatments alone and in combination. first, sixteen peracetic acid-treated samples are exposed to
Advanced therapies, such as the application of peracetic acid X-rays and measured for diffracted intensity at 5–40 degree
(PAA) and irradiation at three kGy, showed higher perfor- angles from Atomic Energy Research and Establishment,
mance in crystallinity, tensile strength, water resistance, and Bangladesh. In the previous study, the resulting impacts
general material characteristics. In contrast, the untreated varied depending on the dosage received. 1.5 kGy, 3 kGy,
jute fibers (Raw JF_TiO2 Coating) served as the baseline. 4.5 kGy, and 6 kGy gamma radiation dosages analysis found
The synergistic effects of combining various treatments that 3 kGy doses of gamma radiation showed considerably
are significantly more significant than the improvements significant changes in the crystallinity of jute fibers [34].
possible with just one technique. The results of this study This study exposed raw jute fibers, cellulose, and those
demonstrate the possibility of combining irradiation meth- treated with peracetic acid (PAA) to gamma irradiation.
ods, chemical changes, and nanomaterial coatings to create
high-performance, environmentally friendly materials from Table 1 % of crystallinity measurement of T
iO2 covered and gamma
natural fibers. irradiated jute fibers
Sample Raw jute Raw Raw Cellu- PAA-
name fibers JF_TiO2 JF_3kGyTiO2 lose JF treated
2 Materials and Methodology coating coating 3 kGy JF_3kGy-
TiO2 TiO2
coating coating
2.1 Materials
% of 60.300 62.546 73.847 77.624 83.533
Jute fiber was purchased from the local market. Other ana- crys-
lytical-grade chemicals, such as peracetic acid, acetic acid, tallin-
ity
Hydrochloric acid, and ethanol, were acquired from Labtex,
Fibers and Polymers
Subsequently, the raw, cellulose, and PAA-treated jute fibers the solution of TiO2 for 2 min. The TiO2-coated yarn was
were coated with T iO2 and then subjected to 3 kGy gamma then dip-coated in the PVA solution for 20 s to bind the T
iO2
irradiation, as this dosage exhibited the highest crystallinity onto the jute surface. Subsequently, all the coated samples
(Table 1). were oven-dried at 80 °C for 1 h and left at room temperature
for 2 h. Coated samples were washed with distilled water to
2.4 Preparation of TiO2 and PVA Suspension remove unfixed T iO2 nanoparticles from the jute yarn. The
samples shown in Fig. 1 were oven-dried at 80 °C for 1 h
A clean beaker was emptied, and 50 mL of 99% absolute and then left under room temperature for 4 h.
ethanol was poured at room temperature. Under magnetic
stirring, 5 mL of titanium isopropoxide (TTIP) was added
drop-wise to the ethanol using a micropipette, forming a 2.6 Evaluation of Water Resistance Properties
milky white solution. After stirring the mixture for 30 min,
hydrochloric acid (HCl) was introduced into the solution to 2.6.1 Moisture Content and Regain
knock out the hydrolysis reaction. Although stirring, HCl
was added drop-wise until the solution turned clear and Moisture content (C) and moisture regain (R) were meas-
transparent. The resulting clear solution was filtrated by fil- ured to assess jute fibers' hygroscopic behavior. Moisture
ter paper and aged for 1 h. content is the percentage of water as compared to the overall
100 mL of distilled water was poured into a beaker and weight of the fiber, whereas moisture regain is the percent-
set on a hot magnetic plate. The 5 g of PVA powder was age of water related to oven-dry weight. Samples were kept
added to water heated to 80–90 °C. The stirring was contin- at 20 ± 2 °C and 65 ± 2% relative humidity for 24 h. The
ued until the PVA wholly dissolved. Afterward, the solution conditioned weight (W + D) was recorded, then oven-dried
was filtered using fine mesh filter paper to remove undis- at 105 ± 2 °C for 2 ± 0.1 h to get the dry weight (D). The
solved particles. Finally, the solution was allowed to cool to moisture content and regain were determined using the fol-
room temperature, as shown in Fig. 1. lowing equations:
The dip-coating method was utilized to pro- Moisture regain, R = W∕D × 100 (2)
duce the TiO2-coated jute fibers. Two beakers containing the
where Oven dry weight of a material = D; Weight of water
solution of T iO2 and PVA were set next to each other. A
in this material = W.
yarn of jute fiber was taken from the sample and dipped in
All procedures were carried out per the ASTM D2654-22 3 Results and Discussion
standard for textile moisture analysis.
3.1 X‑Ray Diffraction (XRD) Analysis
2.6.2 Water Absorption
Figure 2 illustrates the X-ray diffraction patterns of four
The water absorption of fibers was measured as per ASTM types of jute samples. The PAA-treated jute fiber subjected
D570. Fiber specimens (~ 5 g) that had been uniformly cut, to 3 kGy gamma irradiation exhibits the highest intensity,
cleaned and oven-dried were first weighed (M₀). After that, whereas the TiO2-coated raw jute fiber irradiated at 3 kGy
the samples were submerged in room temperature distilled shows the lowest intensity. The other two samples display
water for 10-min intervals for one hour. After immersion, similar intensities, which fall within the moderate range.
the samples were placed between circular metal disks and This suggests that the crystallinity of the jute fibers is pro-
filter papers so excess surface water was eliminated during portional to their diffraction intensity. The X-ray diffraction
immersion, and the wet weight (Mt) was noted. (XRD) analysis revealed significant variations in jute fibers'
crystallinity index (CI) subjected to different treatments,
Water Absorption (%) = (Mt − Mo)∕Mo × 100 (3)
highlighting the influence of T iO2 coating, gamma irradia-
where M0 is the initial mass of the dry specimen, and Mt is tion, and chemical modifications. The untreated T iO2-coated
the mass of the immersed specimen after a specific period. fibers (Raw J F_TiO2 coating) exhibited a baseline crystal-
linity of 62.55%, indicating the inherent semi-crystalline
2.6.3 Water Contact Angle nature of jute fibers. Using better interfacial contact result-
ing from radiation exposure and rearrangement of cellulose
The water contact angle was evaluated using the sessile drop chains, gamma irradiation at 3 kGy raised the crystallinity to
technique and ImageJ software's Axisymmetric Drop Shape 73.85% in Raw JF_3KGY-TiO2-coated fibers. Significantly
analysis profile (ADSA-P). A small droplet of distilled water removing amorphous components and improving structural
was gently deposited on the cleaned and aligned jute fiber alignment, the following chemical treatment with cellulose
surface in a flat configuration. The contact angle was cal-
culated by studying the droplet shape to determine surface
hydrophobicity. Measurements were taken at multiple loca-
tions to verify accuracy, and the average value was given.
This method applies the ideas of Young's equation to deter-
mine surface energy characteristics.
The above Water Resistance testing methodology applied
here is consistent with our previous publication, which used
the same standard testing protocols to evaluate these water
resistance parameters. However, the current study is based
on different fiber TiO2-coated jute fibers—which undergo
additional surface modification through chemical treatment
and gamma irradiation. Although the testing and analysis
procedures remain the same, the surface modifications and
objectives differ. The examined data are listed in Table 2.
Table 2 Analysis of water resistance properties of gamma-irradiated and TiO2 coated jute fibers
Sl. no. Sample name Moisture content Moisture regain Water contact angle Water absorption
(degree)
3.3 Enhancement of Water Resistance Properties the combined effects of TiO2 coating, gamma irradiation,
of Gamma‑Irradiated and Coated Jute Fibers and chemical treatments in significantly enhancing the water
resistance properties of jute fibers.
The analysis of water resistance properties, including The highest water resistance was achieved in the PAA-
moisture content, moisture regain, water absorption, and treated sample (PAA-treated JF_3KGY-TiO2 coating), which
water contact angle, illustrates the progressive enhance- exhibited a moisture content of 3.86%, moisture regain of
ment of hydrophobicity in TiO2-coated jute fibers by apply- 4.01%, and water absorption of 102.26%, alongside a water
ing gamma irradiation and chemical treatments. Untreated contact angle of 86.25°. PAA treatment caused surface
raw jute fibers were highly hydrophilic, as evidenced by crosslinking and structural modification, which improved
their high moisture absorption metrics. The T iO2 coating water resistance, evidenced by the increased contact angle.
alone (Raw JF_TiO2 coating) reduced the moisture content The incorporation of poly-acrylic acid created a highly
to 9.02%, moisture regained to 9.91%, and water absorp- crosslinked and hydrophobic surface, demonstrating the
tion to 169.86% while increasing the water contact angle combined effects of TiO2 coating, gamma irradiation, and
to 45.86°, indicating a slight improvement in water resist- chemical treatments in significantly enhancing the water
ance. Further exposure to 3 Gy gamma irradiation (Raw resistance properties of jute fibers (Fig. 4).
JF_3KGY-TiO2 coating) improved substantially, with mois- As shown in Table 3 depicts the improvement in water
ture content decreasing to 6.24%, moisture regaining to resistance properties of T iO2-coated jute fibers as compared
6.66%, and water absorption to 127.99%. The water contact to raw fibers. Among the coatings, PAA-treated JF_3KGY-
angle rose to 72.25°, reflecting a shift toward hydrophobic TiO2 exhibited the highest reduction in moisture content
behavior due to enhanced surface modification by radiation. (67.54%), moisture regain (70.24%), and water absorption
Chemical treatment (Cellulose JF_3KGY-TiO2 coating) fur- (52.92%), along with a 117.51% increase in water contact
ther decreased moisture content (4.70%), moisture regain angle. This significant enhancement suggests superior hydro-
(4.93%), and water absorption (120.00%), with the water phobicity due to surface modification and improved coat-
contact angle increasing to 76.92°, attributed to the removal ing adhesion. Similarly, cellulose-treated JF_3KGY-TiO2
of hydrophilic amorphous constituents such as lignin and also demonstrated notable reductions in moisture content
hemicellulose. The highest water resistance was achieved (60.43%), moisture regain (63.41%), and water absorption
in the PAA-treated JF_3KGY-TiO2 coating), which exhib- (44.75%), with a 93.98% increase in water contact angle.
ited a moisture content of 3.86%, moisture regain of 4.01%, Raw JF-TiO2 and Raw JF_3KGY-TiO2 coatings showed
and water absorption of 102.26%, alongside a water contact moderate improvements, but their effectiveness was lower
angle of 86.25°. The incorporation of per-acetic acid created than that of chemically treated samples. The bar chart in
a highly crosslinked and hydrophobic surface, demonstrating Fig. 5 visually illustrates this trend, emphasizing the superior
Table 3 Comparison of water resistance properties of gamma-irradiated and TiO2 coated jute fibers with raw jute fibers
Sl. No. Sample name Moisture content Moisture regain Water absorption Water contact
reduction (%) reduction (%) reduction (%) angle increase
(%)
water resistance of PAA-treated JF_3KGY-TiO2, making it caused by radiation point to structural breakdown. Chemical
a promising candidate for moisture-resistant applications. treatments affected the fiber's shape. Lignin and hemicel-
lulose were eliminated to increase surface area and enhance
3.4 Morphology Analysis of the Gamma‑Irradiated coating adherence, producing more refined and porous cel-
and TiO2‑Coated Jute Fibers lulose-extracted fibers. Significant gaps in these fibers point
to improved permeability, although at the cost of mechanical
The structural modifications of jute fibers due to T
iO2 coat- integrity. Fibers treated with PAA showed increased uni-
ing, gamma radiation, and chemical treatments were inves- formity and compactness. The PAA layer reduced micro-
tigated using SEM imaging. Both side-view and end-view cracking brought on by gamma radiation and improved TiO2
analyses provided insights into surface morphology, inter- adhesion. Finally, fiber structure was greatly impacted by
nal porosity, and coating adhesion. Untreated jute fibers chemical treatments and gamma radiation. Although it also
exhibited a relatively smooth yet naturally rough surface brought flaws that can compromise mechanical performance,
with minor impurities. The cross-sectional view revealed a radiation improved porosity and reactivity. Treatment of cel-
dense structure with inherent voids, characteristic of natural lulose reduced fiber density but improved T iO2 penetration.
fibers. Upon T iO2 coating, the fibers showed a thin layer PAA treatment maintains coating adhesion and structural
of deposition with uneven distribution, primarily adhering integrity quite well. These results improve the jute fiber
to the outer surface without significant penetration into the changes for advanced materials' optimization (Figs. 6, 7, 8).
fiber matrix. Increased surface roughness and internal poros- The SEM pictures at magnifications between 1500× and
ity followed by gamma radiation at 3 kGy. The interaction 20,000× thoroughly analyze fiber porosity, T iO2 coating
between fiber and T iO2 improved; nonetheless, the coating's dispersion, and structural integrity. Lower magnifica-
dispersion is not uniform. Microcracks and Delamination tions (1500×–5000×) reveal overall fiber morphology
Fibers and Polymers
Cellulose JF Tio2-3KGY
PAA JF Tio2-3KGY
and coating adherence, whereas medium magnifications 20,000x. The investigation reveals that gamma radiation
(7000×–10,000×) disclose finer pore architectures and increases porosity but causes fiber deterioration, whereas
coating penetration. Nanoscale pores, fiber wall delamina- chemical treatments, especially PAA, improve coating
tion, and T
iO2 aggregation are apparent at a magnification
Fibers and Polymers
uniformity and structural integrity. These findings are cru- The fibers treated with PAA (PAA X10_3KGY-TiO2) exhib-
cial for enhancing fiber changes in composite applications. ited the most uniform and densely arranged TiO2 coating.
The study of particle size revealed an average dimension in
3.5 Particle Analysis of Gamma Irradiated the nanometer range, marked by a narrow size distribution
and TiO2‑Coated Jute Fibers and minimal aggregation. The consistency arises from the
crosslinking action of peracetic acid, which stabilizes par-
The surface morphology and particle distribution of ticle dispersion and enhances adhesion to the fiber surface.
TiO2-coated jute fibers subjected to gamma irradiation were Mountain Software's SEM pictures quantified these find-
analyzed through SEM images processed with Mountain ings by quantifying particle size, distribution uniformity,
Software [37, 38]. The study revealed significant altera- and surface roughness [39]. The treated fibers displayed
tions in the surface morphology and uniformity of the TiO2 a smoother and more homogeneous surface morphology
coating on the fibers across various treatment conditions. than the untreated ones, indicating the synergistic effects of
Untreated fibers exhibited significant aggregation of T iO2 gamma irradiation and chemical treatments in optimizing the
particles, leading to uneven surface coverage. Exposure to TiO2 coating for enhanced performance in Fig. 9.
3 kGy gamma irradiation (Crude JF_3KGY-TiO2) drove There is an inverse relationship between the mean particle
the scattering and grip of TiO2 particles on the fiber surface, distribution area and the crystallinity of T iO2 in gamma-
ascribed to radiation-induced actuation of cellulose, which irradiated jute fibers. While lower crystallinity can lead to
upgraded interfacial interaction between TiO2 and the fiber clustering, which increases the mean particle distribution
lattice. area, higher crystallinity produces finer and more uniformly
The chemical treatment with cellulose (Cellulose distributed particles, which decreases the projected area per
JF_3KGY-TiO2) resulted in smaller and more uniformly dis- particle. Because crystallinity affects nucleation, growth,
tributed TiO2 particles, suggesting a reduction in agglomera- and agglomeration, there is an inverse relationship between
tion. Removing surface contaminants and amorphous com- TiO 2 crystallinity and mean particle distribution area.
ponents through chemical treatment resulted in a cleaner The mean projected area per particle is decreased by the
and more reactive surface conducive to particle adhesion. many tiny, well-separated particles produced by controlled
Fibers and Polymers
(a) (b)
Information Information
Projected Z- Projected Z-
Parameters Parameters
area maximum area maximum
nucleation, which is encouraged by higher crystallinity [40]. crystallinity increases, the particles remain finer and more
On the other hand, irregular growth and particle coalescence uniformly distributed, decreasing the overall mean particle
caused by lower crystallinity result in larger clusters that distribution area (Fig. 10).
raise the mean distribution area. Uneven deposition and Particle density and crystallinity are directly related; bet-
agglomeration result from the absence of distinct nucleation ter dispersion causes higher particle density when crystallin-
sites in amorphous or low-crystallinity TiO2 [41]. Thus, as ity is higher, whereas clustering and coalescence cause lower
Fibers and Polymers
(a) (b)
Information Information
Threshold Threshold
0.4 µm 0.5575 µm
1 1
Projected Z- Projected Z-
Parameters Parameters
Fig. 10 Particle analysis of 3 kGy gamma irradiate as well as TiO2 coated a cellulose and b PAA treated jute fibers
Fibers and Polymers
particle density. While excessive gamma irradiation may result on the water contact angle (WCA) of jute fibers. Rough-
in aggregation, which would marginally reduce density, mod- ness modifies the solid–liquid interface at the microscopic
erate irradiation can increase crystallinity and particle density. level, affecting how water droplets spread or bead up. The
Because crystallinity regulates nucleation, growth, and disper- Wenzel model states that when a surface has a low WCA
sion, there is a direct relationship between T iO2 crystallinity (high hydrophilicity), increased roughness expands the con-
and particle density. A uniform distribution of finely dispersed tact area between the fiber and water, further lowering the
TiO2 particles across the fiber surface is ensured by higher WCA and promoting water absorption. Conversely, rough-
crystallinity, which forms many stable nucleation sites. This ness enhances water repellency on hydrophobic surfaces
raises the particle density by increasing the number of parti- (high WCA) by reducing adhesion [45]. According to the
cles per unit area. On the other hand, irregular nucleation and Wenzel model, when surface roughness creates air pockets
unchecked growth caused by lower crystallinity lead to larger beneath a droplet, water partially rests on trapped air, reduc-
clusters and particle agglomeration, thereby reducing density ing solid–liquid contact and significantly increasing WCA,
by decreasing the number of distinct particles per unit area. leading to superhydrophobic behavior. By altering roughness
Although excessive gamma irradiation can cause defects or at the micro- and nanoscale through T iO2 coatings, gamma
local fusion, which can slightly reduce density by encouraging irradiation, or plasma etching, jute fibers become more
clustering, moderate irradiation improves crystallinity, improv- water-resistant by decreasing surface energy and increasing
ing dispersion and increasing particle density [42]. hydrophobicity [16]. Owing to their effects on wettability,
adhesion, and fiber durability, surface roughness and WCA
3.6 Surface Roughness of the Gamma‑Irradiated are inextricably linked.
and TiO2‑Coated Jute Fibers As per the data, surface roughness and water contact
angle (WCA) in TiO2-coated jute fibers are directly inverse
The surface roughness of TiO2-coated jute fibers, both raw correlated; a decrease in surface roughness causes an
and cellulose-enriched, was analyzed using ISO 25178 increase in WCA, which gives hydrophobicity. The lowest
parameters to evaluate the effects of 3 kGy gamma irradia- value of the water contact angle (WCA) (45.86°) coupled
tion and T iO2 deposition. Average roughness (Sa) Varied with the highest value of surface roughness (0.2736) for the
between 0.1962 and 0.2789 µm, with irradiated cellulose Raw JF_TiO2 coating sample indicates strong water affin-
fibers (SR 4: 0.2789 µm) exhibiting the highest roughness, ity. Gamma irradiation (3KGY) and chemical treatments
likely due to TiO2 nanoparticle agglomeration. Surface lead to increasing crystallinity, and roughness also gradu-
Skewness (Ssk) Predominantly negative (SR 5: − 1.818; SR ally decreases (0.2362 → 0.181 → 0.1418), while WCA sig-
3: − 1.083), indicating valley-dominated topography, benefi- nificantly increases (72.25° → 76.92° → 86.25°), While the
cial for polymer adhesion via mechanical interlocking. The water contact angle (WCA) demonstrates improved water
outlier SR2 (+ 0.2351) suggests localized peak formation, resistance. This pattern is consistent with the Wenzel model,
potentially from uneven coating. Kurtosis (Sku) elevated which states that increased crystallinity and decreased
values (SR 5: 5.217; SR 3: 3.363) highlight sharp peaks/val- roughness reduce direct water-fiber contact and increase
leys, implying heterogeneous surfaces, whereas lower Sku hydrophobicity.
(SR2: 1.562) denotes uniformity. Rougher surfaces enhance Figure 15 shows a substantial association between
interfacial bonding in composites. Valley-dominated profiles enhanced toughness, reduced surface roughness, and higher
improve liquid retention for coatings [43]. Gamma irradia- water contact angle for TiO2-coated jute fibers. The tough-
tion reduced roughness in raw fibers, likely by removing ness of raw fibers increases significantly from 5.791 to
amorphous components. The T iO2 coating and 3 kGy irra- 8.38 J/m3 in PAA-treated ones, indicating better mechani-
diation significantly alter jute fiber surface roughness, with cal integrity. Surface roughness decreases from 0.2736 to
implications for adhesion, wettability, and mechanical per- 0.1418 µm, resulting in smoother, more compact surfaces.
formance. Although most samples exhibit valley-dominated Therefore, surface treatments improve WCA and modify
topography (negative Ssk), outliers like SR2 highlight the roughness, increasing the fibers' resistance to moisture for
importance of process optimization. These findings provide sophisticated uses.
a foundation for tailoring jute fibers for advanced material
applications [44] (Figs. 11, 12, 13, 14). 3.8 Enhancement Mechanical Properties
of the Gamma‑Irradiated and TIO2‑Coated Jute
3.7 Effect of Surface Roughness on Water Contact Fibers
Angle in Tio2‑Coated Jute Fibers
For composites, textiles, and biodegradable materials, jute
The relationship between surface texture and liquid behav- fibers' mechanical qualities, such as their tensile strength,
ior directly influences the impact of surface roughness elongation at break, Young's modulus, and toughness, are
Fibers and Polymers
essential. The cellulose crystallinity, lignin and hemicel- The mechanical properties of jute fibers were significantly
lulose content, and microstructural integrity of the fiber enhanced through TiO2 coating and gamma irradiation,
all affect these characteristics [46]. Strong cellulose fibrils as evident from the increase in breaking force and reduc-
oriented along the fiber axis give jute fibers high tensile tion in extension percentage. The untreated raw jute fibers
strength but are also brittle, resulting in moderate elongation (Raw JF) had the lowest breaking force (232.22 N) with the
at break. Fiber composition and alkali treatment, TiO2 coat- highest extension (3.659%), indicating lower strength and
ing, or gamma irradiation, which can improve crystallinity higher deformability. T iO2 coating (Raw J F_TiO2 coating)
and interfacial bonding in composites, impact Young's mod- increased the breaking force to 367.18 N due to forming a
ulus, which gauges stiffness. Structural homogeneity and protective TiO2 layer, which improved load-bearing capacity
moisture resistance are prerequisites for toughness, which and interfacial bonding. Gamma irradiation at 3 kGy (Raw
is the fiber's capacity to absorb energy before failing [47]. JF_3KGY-TiO2 coating) further enhanced the breaking force
Hydrophobic surface treatments are necessary to preserve to 401.91 N while reducing extension to 3.26%, suggesting
fiber strength because excessive water absorption reduces crosslinking and molecular alignment, which made the fibers
mechanical performance. Strength, flexibility, and durabil- stiffer and more resistant to deformation. Chemical treatment
ity can all be balanced in jute fibers for high-performance (Cellulose JF_3KGY-TiO2 coating) further improved struc-
applications through chemical changes and radiation [48] tural integrity by removing amorphous components, result-
(Fig. 16). ing in a breaking force of 462.29 N and reduced extension to
Fibers and Polymers
2.97%. The most significant enhancement was observed in The stress–strain behavior of jute fibers, which repre-
PAA-treated fibers (PAA X10_3KGY-TiO2 coating), where sents their mechanical response under applied load, con-
the breaking force peaked at 492.23 N, and extension fur- trols the relationship between force and percentage exten-
ther dropped to 2.93%, indicating the most substantial and sion. According to Hooke's Law, the fiber first experiences
most rigid structure. The combined effects of TiO2 coat- elastic deformation when force is applied, during which the
ing, gamma irradiation, and chemical modifications created extension grows proportionately to the force. When the fiber
a more compact, crystalline fiber structure with superior is unloaded in this area, it regains its original shape. Jute fib-
mechanical performance, making these fibers ideal for high- ers move into the plastic deformation region after reaching
strength applications (Table 4). the elastic limit, where molecular chains begin to slip and
Table 5 presents the percentage increase in mechanical cause irreversible elongation.
properties of coated jute fibers compared to raw JF. The As seen in Fig. 18, TiO2 coating and gamma irradiation
PAA-treated JF_3KGY-TiO2 coating showed the highest greatly enhanced the mechanical qualities of jute fibers,
improvement in breaking force (112%), tensile strength as demonstrated by the rise in toughness, elastic modulus,
(169.85%), elastic modulus (237.26%), and toughness and tensile strength. With an elastic modulus of 5.80 GPa
(116%), followed by cellulose-treated JF_3KGY-TiO 2 and a tensile strength of 212.22 MPa, the untreated raw jute
(99.14%, 113.47%, 163.11%, and 73.13%, respectively). fibers (Raw JF) performed the worst mechanically. Owing
Raw JF_3KGY-TiO2 and Raw JF-TiO2 coatings also to the development of a protective layer that enhanced
enhanced mechanical properties but to a lesser extent. The interfacial bonding and load distribution, applying TiO2
significant improvements are attributed to improved interfa- coating (Raw JF_TiO2 coating) increased these values to
cial adhesion, increased fiber rigidity, and better stress dis- 320.81 MPa and 8.89 GPa, respectively. By encouraging
tribution. The bar chart in Fig. 17 visually compares these crosslinking and molecular realignment, gamma irradiation
enhancements, confirming the effectiveness of TiO2 coat- at 3 kGy (Raw JF_3KGY-TiO2 coating) further reinforced
ings and surface modifications in reinforcing jute fiber for the fibers, raising their modulus to 11.71 GPa and tensile
advanced application. strength to 359.09 MPa. Amorphous components were
Fibers and Polymers
Fig. 13 Surface roughness analysis of the TiO2-coated 3 kGy irradiate raw jute fibers
100
Toughness, J/m3
90
Water contact angle (degree)
80
70
60
50
40
30
20
10
0
Raw JF_TiO2 coa ng Raw JF_3KGY-TiO2 Cellulose JF_3GKY-TiO2 PAA X10_3KGY-TiO2
(a) coa ng coa ng coa ng
(b) (c)
Fig. 15 Surface roughness analysis of the TiO2-coated 3 kGy irradiate raw jute fibers
eliminated by chemical treatment (Cellulose JF_3KGY-TiO2 peracetic acid (PAA) treatment, gamma irradiation, and
coating), resulting in a more compact and crystalline fiber TiO2 nanoparticle coating. Every level of alteration made
structure with an impressive tensile strength of 452.83 MPa a unique contribution: chemical treatments changed the
and a modulus of 15.26 [Link] strong hydrogen bond- internal structure by eliminating amorphous components,
ing and crosslinked network formed by poly-acrylic acid allowing deeper penetration of nanoparticles; gamma irra-
markedly improved fiber reinforcing. The most remarkable diation encouraged crosslinking and interfacial bonding;
improvement was seen in the PAA-treated fibers (PAA- and TiO2 coating enhanced surface reactivity. Among all
treated 3KGY-TiO2 coating), achieving a tensile strength the treatments, PAA produced the best fiber transformation,
of 572.58 MPa and an elastic modulus of 19.56 GPa. The creating a uniform and compact surface that enhanced TiO2
enhanced stiffness and longevity of the fibers are evident via adherence and reduced irradiation-induced microcracking.
the steady decrease in strain and elongation, making them This combination, supported by improved crystallinity and
ideal for high-performance applications. changed surface chemistry, produced greater mechanical
strength, structural integrity, and water resistance.
These results highlight the usefulness of this hybrid mod-
4 Conclusion and Future Work ification technique in creating long-lasting, environmentally
friendly materials based on jute fiber for cutting-edge pack-
To significantly improve the performance of jute fibers, this aging, composites, and functional fabrics. More research
study offers a thorough and integrated treatment approach into maximizing PAA concentration and irradiation dosage
that includes chemical surface modification, specifically is necessary to finetune the fiber properties. Confirming the
Fibers and Polymers
(a) (b)
(c) (d)
Fig. 16 Enhancement of the force and extension % a without gamma irradiated raw b 3 kGy gamma irradiated raw c 3 kGy gamma irradiated
cellulose d 3 kGy gamma irradiated PAA treated, TiO2 coated jute fibers
Table 5 Percentage increase in breaking force, tensile strength, elastic modulus, and toughness
Sl. no. Sample name % Increase in break- % Increase in tensile % Increase in elastic % Increase
ing force strength modulus in toughness
100
50
0
% Increase in % Increase in Tensile % Increase in Elasc % Increase in
Breaking Force Strength Modulus Toughness
changed fibers' industrial feasibility will also require assess- produced a dense and homogenous structure enhancing
ing their long-term performance and biodegradability in TiO2 adhesion and reducing the negative impacts of gamma
various environmental settings. radiation-induced micro-cracking. The PAA-treated fibers
Using TiO2 coating, gamma irradiation, and chemical showed improved performance and the highest degrees of
treatments, this study has demonstrated notable improve- mechanical strength, stiffness, toughness, and water resist-
ments in jute fibers' mechanical properties and water resist- ance. The observed improvements in crystallinity and com-
ance. The progressively better results of every treatment bined changes in surface form and chemical composition
phase emphasize the combinatorial effects of these changes. support the success of the combined treatment approach.
Early results came from applying TiO2 coating, yet gamma The findings show that PAA treatment combined with TiO2
irradiation greatly improved fiber properties, most likely by coating and gamma irradiation provides a practical approach
allowing crosslinking and increasing fiber–TiO2 interaction. for producing high-performance jute fiber-based materials in
Changing the fiber structure was primarily dependent on packaging, textiles, and composites. Future studies should
chemical treatments. Eliminating lignin and hemicellulose focus on raising PAA content and gamma irradiation dosage
enhanced TiO2 penetration; nevertheless, increased poros- to improve fiber properties and assess the long-term durabil-
ity may have compromised the mechanical integrity of the ity of treated fibers in many environmental conditions.
fiber. The most effective method was PAA treatment, which
Fibers and Polymers
(a) (b)
(c) (d)
Fig. 18 Enhancement of tensile stress, elastic modulus concerning strain a without gamma irradiated raw b 3 kGy gamma irradiated raw c 3 kGy
gamma irradiated cellulose d 3 kGy gamma irradiated PAA treated, TiO2 coated jute fibers
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