Effect of TiO 2 nanoparticle reinforcement on the mechanical and tribological performance of natural fiber hybrid polymer composites

Abstract

Particle reinforcement is one of the methods used in natural hybrid composite manufacturing to enhance mechanical characteristics. In this work, four distinct hybrid laminates were prepared using natural fibers and four different weight percentages (Wt.%) of titanium oxide nano filler by the compression molding procedure. Epoxy served as the matrix, and sisal and banana fibers were utilized as natural reinforcements. With the addition of the hybrid fiber reinforcement and TiO₂ filler, the mechanical properties of flexural, impact, and tensile characteristics improved greatly (impact energy of 13.452 J, flexural strength of 94.86 MPa, and tensile strength of 18.6 MPa). Mechanical performance was enhanced in polymer-based composites by the addition of 3 Wt. % TiO₂ filler. The features are improved by the filler substitutes, which fill the space between the fiber and matrix phases. When 3 weight percent TiO₂ (T3) was added, the minimum wear of 13 μm with the Coefficient of Friction 0.0068 was observed for the T3 at a 20 N load, with a frictional force of 0.2 N.

Keywords

titanium oxide mechanical properties coefficient of friction banana fiber sisal fiber

Introduction

Researchers are interested in using natural fibers (NF), which are renewable and sustainable resources, as reinforcement in polymers to replace synthetic fibers. Hydrophobic characteristics are typically found in polymers, whereas hydrophilic characteristics are seen in NF. Due to the advantages of these materials, the automotive industry and others have become increasingly interested in them. NF composites present numerous benefits compared to synthetic fiber composites, including affordability, biodegradability, reduced density, satisfactory specific properties, insulation, improved thermal characteristics, and lower energy usage in processing, among others.¹ Banana is a lignocellulosic fiber sourced from the stem of the plant, known for its superior mechanical characteristics. Additionally, among the 130 nations that grow bananas, India stands as the top producer, accounting for 27% of global production. Karnataka is one of the leading states in India for banana cultivation. Bananas are also grown in several states of South India, such as Tamil Nadu (TN), Maharashtra (MH), Kerala (KL), and Andhra Pradesh (AP). Similarly, they are also grown in Northeast India, including Assam (AS) and Gujarat (GJ). Banana fibers (BF) are a byproduct of their cultivation; therefore, the source can be accessed for industrial uses without any investment. Numerous studies have examined natural fibers for various purposes due to their suitable stiffness, excellent disposability, and renewability. Additionally, they can be recycled and are capable of biodegradation. Plant fibers are naturally hydrophilic, containing approximately 8–13% moisture and featuring cellulose within their cell structure. Besides cellulose, plant fibers are composed of various natural components, including lignin, hemicellulose, pectin, and waxy substances. The amount of lignin in plant fiber affects its structure, characteristics, and form.² Banana fibers demonstrate significant tensile strength and minimal elongation before breaking. Consequently, utilizing these fibers to prepare hybrid composites as a reinforcement in resin-based composites may offer new opportunities in various fields such as automobile, Civil, and engineering applications. Banana cultivation is highly favored in India; the ability to reuse these pseudo stems could greatly benefit the economy.³ The sisal plant belongs to the Agavaceae family, which produces stiff fibers typically used in the production of twine and rope. These fibers are entirely biodegradable, a renewable energy source, remarkably robust, and easy to maintain, exhibiting minimal wear and tear resistance. Sisal fiber (SF) serves as an excellent raw material for manufacturing natural fiber composites (NFCs). Many NFCs are densely packed with natural fibers to reduce product costs, resulting in a poor interfacial relationship between the fibers and the soft matrix. To properly construct an enhanced performance in NFC, the primary issue that must be addressed is interfacial compatibility. SF is a type of perennial tropical natural fiber distinguished by a high aspect ratio, better stiffness, and robust texture with greater tensile strength and resistance to friction. Generally, products such as carpets, ropes, burlap bags, textiles, and paper. The usage of SF in these items is modest and provides little extra benefit. SF can be used to make NFCs, which is one of the most valuable uses expanding quickly recently.⁴ Among the various natural fibers, sisal and banana exhibit excellent mechanical characteristics.⁵ Epoxy resin is widely utilized as the matrix substance in creating NFC for various structural and industrial uses due to its improved dimensional stability, excellent adhesion, and high resistance to chemicals and heat.⁶ Since using this epoxy as a matrix, which is used to improve the mechanical, thermal, and electrical qualities of the NFC. The introduction of nano fillers promotes the interfacial adhesion and load transfer among composite components, resulting in exceptional mechanical properties.⁷

The hybridization of NF was employed to address limitations such as reduced tensile, flexural, and impact strengths. In recent years, nano-reinforcements have been added to conventional ablative composite materials to achieve property improvements.^8–10 According to recent studies, the mechanical features and abrasive qualities of the NFCs are greatly improved by nano fillers. With nano TiO₂ filler, the mechanical properties of the carbon epoxy composite (CEC) were enhanced because the filler is more rigid than the matrix. The higher the filler supply %, the more difficult the CEC becomes. At all abrading distances, regardless of load intensity, the inclusion of nano TiO₂ decreased the wear loss of the CEC.TiO₂ nano filler, which displays less wear loss than unfilled CE composites, also shows a similar pattern as abrading distance and load increase. When filler is added, the CE composite’s wear rate lowers at both loads because the hard filler particles reinforce the bond between the fiber and the filler-filled matrix and prevent carbon fracture. Incorporating nano TiO₂ filler increases the tensile strength and hardness of CE composites while decreasing wear loss. The mechanical and vibrational characteristics of pineapple, banana, and sisal fibers were enhanced by the application of chemically produced titanium oxide (TiO₂) nanopowder.¹¹ The filler content is the most important factor determining the wear rate, followed by the sliding velocity, according to research on the sliding wear behavior of waste glass dust-filled hemp-epoxy composites and the application of prediction models for the wear study.¹² The tensile, impact, and flexural strengths of hybrid pineapple/sisal, sisal/banana, and banana/pineapple combinations were enhanced by up to 3% TiO₂ replacement. At 4%, uneven nano-filler dispersion reduces the mechanical stability of bio-composites. Because of the enhanced surface contact with the resin/hybrid natural fibers and the filler/resin interface, which results in improved composite stiffness and natural frequency, hybrid combinations of pineapple and sisal with 3% TiO₂ filler had the greatest natural frequency. Natural frequency and damping characteristics improved by incorporating nano-fillers. Wear and deformation behavior is shown to depend strongly on loading conditions, material structure, and composition, with cyclic stresses causing progressive viscoplastic strain accumulation in HDPE-glass fiber composites, particularly in matrix regions between closely spaced fibers. Granular materials exhibit shape-dependent contact orientations, influencing frictional resistance and wear pathways, while higher-order fabric tensors improve the prediction of these anisotropic behaviors.^13–17 The aspects like friction characteristics and energy loss at the peak strain zone in the filler enhance the damping behavior of natural composites.¹⁸ The impact of titanium dioxide (TiO₂) particles as a filler material on the dry slide wear performance of natural Ficus Benghalensis (FB) fiber-reinforced hybrid polymer composites has been studied. The sliding distance and normal load had very little effect on the sliding wear rate, whereas the fiber content had the biggest impact, followed by the sliding velocity. The possibility of using TiO₂ as a filler to enhance the mechanical and wear characteristics of Ficus Benghalensis/epoxy matrix composites.¹⁹ When Sisal/Pineapple fiber reinforcement (1:1 ratio) and TiO₂ filler were added, the mechanical properties of flexural, impact, and tensile characteristics significantly improved. The mechanical performance of the 40 Wt. % Sisal pineapple and 5 Wt.% TiO₂ mixture was enhanced. The addition of a high TiO₂ filler (5 weight percent) to the polymer-based composites resulted in a lower Specific Wear Rate (SWR), according to the Taguchi optimization results. By filling in the gaps between the fiber and matrix phases, the filler substitutes enhance the characteristics.²⁰ The graphene acts as a nano-filler to improve the mechanical properties of hybrid polymer matrix composites reinforced with cotton/viscose fabric. The NFC with banana/jute fiber using a compression moulding technique with rice husk filler percentages of 1-3 Wt.%. The mechanical properties of the hybrid composite were enhanced through the addition of rice husk as a filler. The inclusion of 3 Wt. % of rice husks yields the highest tensile strength and tensile modulus.²¹ This study aims to evaluate the impact of the TiO₂ nano filler on the mechanical and wear properties of banana/sisal hybrid composites fabricated via compression molding with epoxy as the matrix. By incorporating varying weight percentages of TiO₂, the research seeks to enhance interfacial bonding, improving tensile, flexural, and impact strengths, as well as wear resistance and frictional behavior. The work also investigates the TiO₂ loading to maximize performance while analyzing fracture surfaces to understand failure mechanisms. Ultimately, this study demonstrates that TiO₂ nano filler significantly improves the durability and mechanical characteristics of natural fiber composites, promoting their sustainable use in industrial applications.

Preparing TiO₂ filler hybrid composite

Banana and Sisal fibers served as the reinforcement, which were cut into 300 mm × 300 mm pieces from the continuous material. Epoxy (LY556) and hardener (HY951) were utilized as the matrix material. TiO₂ was chosen as the filler material at concentrations of 1 Wt. %, 2 Wt. %, 3 Wt. %, and 4 Wt. %. The TiO₂ has been supplied by Go Green products, Chennai, India, and the properties are listed in Table 1. Two methods were used to add titanium oxide filler to epoxy resin. The first step is mechanical agitation; in this case, the necessary epoxy was added to the nano-TiO2/acetone mixture and agitated for 30 minutes using a mechanical stirrer. An additional 30 minutes of ultrasonication is the next step. After cooling to room temperature, the nano-TiO2/epoxy mixture was combined with the hardener at a 10:1 ratio.²² The fabrication process uses a combination of 0° and 90° orientations for the laying of the laminates. The compression molding process was altered for the experiment to include 40% weight ratio hybrid fiber blends. A weight percentage of nano-TiO₂/epoxy solution is needed to fill the mold containing the hybrid banana/sisal set. With dimensions of 300*300*5 mm, this compression mold creates hybrid composites at 100 °C and 30 MPa of pressure for 1 hour, then allows them to cure to room temperature (24 Hours).²² The required test samples have been prepared from the hybrid Banana and Sisal/TiO₂ for further characterization. Banana and Sisal fibers served as the reinforcement, which were cut into 300 mm × 300 mm from the continuous one. The orientations considered are 0° and 90°.

Table 1.

Properties of TiO₂.

TiO₂	Description
PURITY	>99%
AVERAGE PARTICLE SIZE	<100 nm
PHYSICAL FORM	POWDER
SSA	150 m²/g
BULK DENSITY	0.9 g/cm³
CAS NO	13463-67-7
MORPHOLOGY OF NANO PARTICLE	NEAR SPHERICAL
COLOUR	WHITE

Testing of composites

A Charpy Impact Tester was used to determine the impact strength of hybrid natural composites, while a Universal Testing Machine (UTM) was used for tensile and flexural tests. ASTM D 638, ASTM D 790, and ASTM D 256 standards were used for tensile, flexural, and impact tests. A dumbbell specimen with a gauge length of 50 mm and a crosshead speed of 2 mm/min was used for a tensile test. Flexural and impact tests were performed using a rectangular workpiece with dimensions of 125 × 13 × 3 mm. The wear and friction properties of the produced hybrid NFC were investigated using a pin-on-disc machine with a disc diameter of 150 mm and a track diameter of 100 mm. The ASTM G99 standard was followed in conducting the test, and silicon carbide abrasive paper of grade 1200 was used to polish the testing specimen’s counter face (65 × 13 × 3 mm).²³ Each combination was examined three times.

Coefficient of Friction (μ) = \frac{Measured Frictional Force}{Normal Applied Load}

To identify the structure and existence of TiO₂ nano-powder, SEM testing was performed using the QUANTA 200 MODEL machine from ICON ANALYTICAL.

Results and discussion

The mechanical tests were conducted for the prepared composite with different Wt.% of TiO₂ and Banana/sisal hybrid fiber, revealing the subsequent outcomes (Table 2). According to the results, the inclusion of TiO₂ filler significantly increased the material’s mechanical characteristics. A tensile strength of 11.66 MPa was achieved (Figure 1) by preparing the hybrid composite with 1% TiO₂ (T1). The tensile strength is 14.4 MPa when 2 weight percent of TiO₂ (T2) is added. This indicates a 23.04 % increase in tensile strength in T2. It has been noted that the tensile strength rises with the incorporation of TiO₂; further, the addition of 3 Wt.% of TiO₂ shows the maximum tensile strength of 18.6 MPa, providing an improvement of 36.06 %.

Table 2.

Mechanical properties of TiO2 hybrid composite.

wt. (%)	Tensile strength (MPa)	Flexural strength (MPa)	Impact energy (J)	Shore D hardness
1 Wt.% of TiO₂ (T1)	11.66	66.90	7.909	54
2 Wt.% of TiO₂ (T2)	14.4	82.62	11.325	74
3 Wt.% of TiO₂ (T3)	18.6	94.86	13.452	79
4 Wt.% of TiO₂ (T4)	16.06	83.95	7.909	58

Figure 1.

Tensile and Flexural properties of TiO₂ hybrid composites.

The tensile strength is increased by adding TiO₂ as secondary reinforcement, as the TiO₂ nanoparticles are hard.¹¹ A decrease in tensile strength was noticed for the 4 Wt.% TiO₂ (T4) of 16.06 MPa. A decrease in wettability, leading to a sticking characteristic known as agglomeration, above 3% filler, exhibited a decline in the tensile properties of NFC.²⁴ The combination of 3 Wt.% TiO₂ showed tensile strength. The inclusion of nano fillers decreases the void space between the natural fiber and the epoxy matrix, thereby enhancing the tensile properties of the composite.²⁴ The mechanical characteristics of the banana/sisal fiber-reinforced hybrid composite were improved by using TiO₂. The incorporation of TiO₂ boosts the surface area of the matrix material, resulting in an interfacial bond between the fiber and the matrix.²¹ The smaller particle size of the filler leads to better adhesion and interfacial stiffness, which improves stress transfer and elastic deformation in NFC, thereby enhancing their tensile properties.²⁵ The addition of sugarcane bagasse ash nano fillers up to 5 Wt.% results in a uniform distribution of filler within the sisal, flax, banana, and kenaf natural fiber/epoxy matrix blend.²⁴ The addition of filler also improves flexural properties. The composites experienced enhanced stress transfer due to robust bonding between the fibers and matrix, enabling elastic deformation. The maximum flexural strength is observed at 3 Wt.% of TiO₂ addition of 94.86 MPa. Agglomeration leads to a decrease in flexural properties when nano addition exceeds 3 Wt.%.²⁴ Strong hydrogen bonds were formed because of the epoxy matrix’s higher polarity, which enhanced the hybrid natural composites’ flexural qualities. Viscosity increases with higher filler replacement at higher weight percentages, activating internal component porosities and reducing flexural characteristics.²⁶

The Void content analysis (ASTM D2734) and the density measurements (ASTM D792 – Water Displacement Method) are performed, and the values are provided in Table 3. The addition of TiO₂ strengthens the microstructural interpretation of fiber–matrix interaction. Experimental densities increase gradually with TiO₂ content. Void content remains low across all formulations, confirming good-quality laminate fabrication. A small reduction in void content with increased TiO₂ suggests that nanoparticle reinforcement promotes better resin infiltration and improved interfacial adhesion.

Table 3.

Void validation.

Type	TiO₂ Wt. %	Theoretical density (g/cm³)	Actual density (g/cm³)	Volume fraction of voids
T1	1%	1.211	1.151	4.955
T2	2%	1.22	1.161	4.836
T3	3%	1.228	1.172	4.560
T4	4%	1.237	1.181	4.527

The greatest improvement in impact strength characteristics (Figure 2) was noted at T3, 13.45 J, and the same combination also produced the highest hardness of 79 (Figure 3). This demonstrated the importance of incorporating TIO2 filler in improving the mechanical properties of epoxy-based polymer composites.

Figure 2.

Impact results for different Wt% of Tio2.

Figure 3.

Hardness results.

The fiber pullout was observed in Figure 4 of T1. The T3 combinations achieve a result with enhanced bonding between fiber and matrix, with less fiber pullout, resulting in improved properties. The SEM results demonstrated improvements in morphological features due to the nano-filler incorporation. The SEM results demonstrated improvements in morphological features resulting from the incorporation of nano-fillers. The addition of filler decreases the pores between the reinforcement and matrix phases, thereby improving the compatibility of the polymer-based composite.¹⁸

Figure 4.

SEM analysis after tensile test of T1, T2, T3, and T4.

The inclusion of filler improves the bonding strength between reinforcements and epoxy-based composites. The mix of fiber reinforcements provided sufficient adhesion to the epoxy matrix, enhancing the wear resistance of NFC. 2²⁷ The incorporation of nanoparticles markedly demonstrated beneficial properties for biobased fibers, improving their usability.²⁸

The wear properties (Table 4) of the 4 different composites, such as T1, T2, T3, and T4, have been analysed with the input parameters such as load, speed, and frictional force. From the analysis, the maximum Coefficient of Friction of 0.68 was observed with T2 with a 30 N load, 400 rpm speed, and the frictional force of 0.1 N. The minimum wear 13 μm with the Coefficient of Friction (COF) 0.0068 was observed for the T3 at 20 N load, with the frictional force of 0.2 N. Wear increases directly with applied load, because higher load raises the real contact pressure, accelerates surface damage, and promotes deeper penetration and breakdown of the material.¹⁷ Elevated load formed a highly pressurized area within the composite specimen, leading to increased wear. The calculated COF values were low (0.003–0.031) and showed a decreasing trend with increasing load, indicating effective transfer film formation and stable sliding behavior typical of polymer and polymer composite tribo systems. The enhanced adhesion among fiber reinforcement/TiO₂ filler/epoxy resin forms a tribolayer surface, reducing the interaction between the pin on the disc and the specimen’s surface.²⁰ At lower loads, asperity contact is unstable, and the transfer film is discontinuous, resulting in higher interfacial shear resistance. With increasing normal load, plastic deformation at the asperity tips enlarges the real contact area and promotes the adhesion and compaction of a stable transfer film on the counter face. This transfer layer acts as a protective third-body lubricating film with lower shear strength than the bulk polymer, thereby reducing the coefficient of friction. As per tribological theory, the ability of the material to create a uniform low-shear transfer layer directly correlates with friction reduction during sliding.^29,30 Additionally, TiO₂ nanoparticles dispersed within the matrix contribute to the stability of this film by improving load-bearing capability and preventing severe micro-ploughing. At optimal filler loadings (2–3 wt.% TiO₂), the nanoparticles suppress severe adhesive wear and enhance film integrity. Consequently, the reduction in COF with rising load is consistent with classical friction theories where higher contact pressures facilitate more uniform film formation and reduce adhesive friction.

Table 4.

Wear test results.

Trials	TiO2 Wt.%	Load (N)	Speed (rpm)	Time (sec)	Frictional force (N)	Coefficient of friction (μ)	Wear (μm)
1	1	10	400	500	0.1	0.0102	22
2		20	400	500	0.1	0.0051	47
3		30	400	500	0.2	0.0068	58
4	2	10	400	500	0.3	0.0306	46
5		20	400	500	0.3	0.0153	62
6		30	400	500	0.1	0.0034	68
7	3	10	400	500	0.1	0.0102	42
8		20	400	500	0.2	0.0102	18
9		30	400	500	0.2	0.0068	13
10	4	10	400	500	0.1	0.0102	24
11		20	400	500	0.2	0.0102	61
12		30	400	500	0.2	0.0068	36

Statistical evaluation of the wear and coefficient of friction data reveals clear performance differences among the tested samples (Table 5). T3 exhibits the lowest mean wear depth (24.33 µm), confirming its superior wear resistance compared to the other combinations. Although moderate scatter is observed (standard deviation of 15.50 µm), this variation is attributed to load-dependent transitions in wear mechanisms rather than experimental inconsistency. In contrast, T2 shows the highest mean wear (58.67 µm) along with the largest variation in COF, indicating unstable tribological behavior and poor interfacial control. T1 and T4 demonstrate intermediate wear performance with higher standard deviations, suggesting mixed adhesive–abrasive wear regimes. The relatively low standard deviation of COF for Sets 3 and 4 indicates stable sliding conditions governed by transfer-film formation. Overall, the combination of the lowest mean wear, low average COF, and controlled variability statistically confirms that Set 3 provides the most reliable and tribologically stable performance among all tested samples.

Table 5.

Statistical analysis of wear and coefficient of friction.

Type	Mean Wear (µm)	Std. Dev. (µm)	Mean COF	Std. Dev.
T1	42.33	18.45	0.0074	0.0026
T2	58.67	11.37	0.0164	0.0136
T3	24.33	15.50	0.0091	0.0020
T4	40.33	18.88	0.0091	0.0020

Practical implications

The observed enhancement in tensile, flexural, impact, and hardness characteristics at 2–3 Wt. % TiO₂ suggests that the developed banana/sisal hybrid composites can be considered for lightweight and semi-structural applications. The combination of reduced wear rate and improved hardness supports potential use in tribological components, such as low-load bearings, sliding pads, domestic appliance parts, and automotive interior elements, where a balance between strength, durability, and sustainability is required. The use of naturally derived fibers also aligns with the current industrial trend toward low-density, renewable, and biodegradable composite materials.

Future work

Fiber surface modification to further enhance fiber–matrix bonding

Long-term durability studies, including moisture conditioning, UV exposure, and thermo-oxidative aging.

Fatigue and creep testing to evaluate performance under repeated or sustained loading conditions.

Hybrid reinforcement strategies, combining TiO₂ nanoparticles with other nano/micro fillers to optimize multi-functional performance.

Wear surface morphology to enhance the depth of tribological evaluation.

Conclusion

The hybrid composite of banana and sisal fibers with different TiO₂ fillers has been prepared, and the following mechanical and wear properties have been evaluated.

• The particle reinforcement of TiO2 filler in the hybrid banana/sisal composition resulted in a significant improvement in tensile, flexural, and impact properties.

• The 3 wt.% TiO2 addition (T3) resulted in maximum mechanical parameters, including tensile strength of 18.6 MPa, flexural strength of 94.86 MPa, and impact strength of 13.452

• The agglomeration effect harms the properties of the hybrid composites at the higher level of particle reinforcement (T4).

• The minimum wear of 13 μm with the Coefficient of Friction 0.0068 was observed for T3 at a 20 N load, with a frictional force of 0.2 N.

Footnotes

ORCID iDs

Arunkumar Kuppuraj

Krishnaraj Ramaswamy

Funding

The authors received no financial support for the research, authorship, and/or publication of this article.

Declaration of conflicting interests

The authors declared no potential conflicts of interest with respect to the research, authorship, and/or publication of this article.

Data Availability Statement

The datasets used and analyzed during the current study are available from the corresponding author on request.*

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Effect of TiO 2 nanoparticle reinforcement on the mechanical and tribological performance of natural fiber hybrid polymer composites

Abstract

Keywords

Introduction

Preparing TiO2 filler hybrid composite

Testing of composites

Results and discussion

Practical implications

Future work

Conclusion

Footnotes

ORCID iDs

Funding

Declaration of conflicting interests

Data Availability Statement

References

Preparing TiO₂ filler hybrid composite