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Die Studie konzentriert sich auf die Entwicklung elektrogesponnener PVC- / Graphen-Verbundnanosonden zur Beseitigung von Ölverschmutzungen, wobei die außergewöhnlichen mechanischen Eigenschaften und die hohe Ölaufnahmekapazität von Graphen genutzt werden. Die Forschung untersucht die Optimierung der Graphenkonzentration, um die Zugfestigkeit und die Effizienz der Ölaufnahme zu verbessern, und zeigt signifikante Verbesserungen der mechanischen Leistung und der Umweltverträglichkeit. Der innovative Ansatz, Graphen in PVC-Nanofasern zu integrieren, bietet vielversprechende Lösungen für die Sanierung von Ölaustritten und andere ökologische Herausforderungen und macht diesen Artikel zu einer wertvollen Ressource für diejenigen, die sich für fortschrittliche Materialien und Umwelttechnologien interessieren.
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Abstract
Oil spills in aquatic environments are catastrophic events that pose a significant global environmental challenge. This study addresses these issues by developing innovative poly(vinyl chloride) (PVC) nanofiber mats enhanced with nanographene particles, leveraging their exceptional surface area and unique graphene properties. Recent advances in graphene technology have highlighted its versatility in various fields; however, this work uniquely applies these advancements to oil spill remediation. Embedding nanographene particles into PVC nanofibers using electrospinning resulted in a significant enhancement in mechanical properties and functionality. The nanographene particles were synthesized and incorporated into an aqueous PVC solution at varying concentrations (0.5%, 1%, 1.5%, and 2% by weight). The electrospinning technology produced PVC nanofibers with graphene, resulting in nano-rough surfaces, as revealed by scanning electron microscopy. The nanofiber mats exhibited a remarkable 210% increase in tensile strength at a graphene concentration of 1.5% compared to pure PVC mats, demonstrating the enhanced mechanical performance of the material. Moreover, these nanocomposites exhibited improved oil-spreading kinetics, positioning them highly effective for oil sorption applications. This study presents a novel integration of graphene and PVC nanofibers to create multifunctional materials tailored for environmental remediation. This highlights the potential of nanographene to significantly enhance the mechanical and functional properties of PVC nanofibers, thereby providing a foundation for future advancements in hybrid nanocomposite materials for sustainable and practical applications.
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1 Introduction
The fabrication and investigation of nanographene particles/poly(vinyl chloride) (PVC) nanofiber composites are pivotal for advancing lightweight, high-performance materials. Graphene, recognized for its exceptional mechanical properties, such as high tensile strength and flexibility, enhances polymer composites by improving strength, elasticity, and thermal stability. These characteristics make graphene-reinforced composites suitable for diverse applications, including filtration, energy storage, and biomedical engineering [1‐5]. Recent studies highlight the potential of graphene nanoparticles in improving the tensile strength and flexibility of PVC nanofibers, offering promising opportunities for lightweight yet durable materials in industries like aerospace, automotive, and electronics [6‐8]. Multiple studies have shown that graphene-reinforced polymer composites exhibit an approximately 50% increase in tensile strength even at low graphene content [1]. Poly(vinyl alcohol)/graphene oxide composite fibers demonstrated a notable enhancement, with tensile strength improving by over 120% compared to fibers without reinforcement [9]. Similarly, the addition of graphene nanoplatelets to chitosan/polyvinyl alcohol nanofibers increased tensile strength by 85% while preserving their flexibility [10]. Electrospinning has emerged as a reliable method for fabricating graphene/PVC nanofiber composites, enabling precise control over material morphology to achieve superior mechanical properties [9‐11]. This method facilitates the production of composites with enhanced strength-to-weight ratios, ideal for applications such as flexible electronics, sensors, and battery electrodes [12‐14]. While graphene’s incorporation significantly improves mechanical and thermal properties, achieving uniform dispersion within the PVC matrix remains a challenge. Poor dispersion can lead to agglomeration, negatively impacting mechanical and electrical properties. The techniques such as sonication exfoliation and controlled graphene oxide integration have shown promise in addressing these issues, optimizing the balance between tensile strength and flexibility [15‐18]. These quantitative insights provide a stronger foundation for discussing the mechanical property enhancements observed in graphene/PVC nanofiber composites and align with the findings of the current study. This addition underscores the novelty and significance of our work while situating it within the broader context of related research.
Polyvinyl chloride (PVC) combined with graphene nanocomposites has emerged as a promising material for oil spill remediation due to its unique properties. The integration of graphene into PVC enhances the material’s mechanical strength, chemical resistance, and adsorption capacity, making it highly effective in separating oil from water [19, 20]. This combination leverages the superhydrophobic and oleophilic nature of graphene, which allows for efficient oil absorption while repelling water. The development of PVC/graphene nanocomposites represents a significant advancement in environmental technology, offering a sustainable and efficient solution for mitigating the detrimental effects of oil spills on marine ecosystems. Poly(vinyl chloride) (PVC)/graphene nanocomposites offer a unique combination of mechanical strength, flexibility, and surface roughness, making them highly effective for environmental applications such as oil spill remediation [1]. The hydrophobic nature of graphene enhances the sorption capacity of the composite, while PVC provides a robust structural matrix for long-term performance. The studies have demonstrated that graphene-based materials, with their high specific surface area and oleophilic properties, can significantly improve oil absorption efficiency [21, 22]. Moreover, the use of poly(vinyl chloride) as a base polymer enhances the durability and reusability of the composite, ensuring its practicality for large-scale deployment [10, 12]. Incorporating graphene nanoplatelets into PVC nanofibers has created nanoroughness on the fiber surface, further enhancing oil-spreading dynamics and sorption capacity, as reported [23, 24]. This makes PVC/graphene nanocomposites particularly promising for addressing aquatic oil spill challenges, offering an eco-friendly and efficient alternative to conventional materials.
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Graphene, known for its exceptional properties such as high electrical and thermal conductivity, remarkable mechanical strength, and flexibility, is synthesized using various methods. These methods include chemical vapor deposition (CVD), mechanical exfoliation, chemical reduction of graphene oxide, and liquid-phase exfoliation. Each technique has its advantages and challenges. For instance, CVD produces high-quality graphene suitable for electronics, while liquid-phase exfoliation is efficient for large-scale production [25]. This research stands out by incorporating advanced material synthesis techniques, specifically the nanographene particles creation and their uniform distribution within PVC solutions, to develop hybrid nanocomposite materials. Additionally, it emphasizes the significant potential of these nanocomposite mats to innovate oil sorption applications, merging high durability and efficiency without sacrificing PVC’s inherent properties.
Integrating PVC polymer nanofibers with nanographene notably improves the mechanical properties and functional potential of electrospun fibrous mats. This enhancement is evident through improved tensile strength, increased Young’s modulus, and better oil absorption capacity. Incorporating nanographene particles into PVC nanofibers reinforces the material but also introduces unique properties such as higher surface area and improved pore structure, making them highly effective for applications like oil spill remediation and filtration membranes. This innovative approach leverages the strengths of both materials, resulting in advanced nanocomposites with vast potential in various technological fields [26‐28].
The investigation examines the effects of varying graphene concentrations in PVC nanofibers, employing electrolysis and exfoliation to produce nanographene. The results reveal valuable insights into the relationship between graphene content and the mechanical properties of nanofibers, underscoring their potential in applications such as oil absorption. This work advances the synthesis and characterization of graphene-reinforced composites, contributing to the creation of multifunctional materials for emerging technologies. The study’s dual focus on enhancing mechanical performance and oil spill mitigation positions it as a noteworthy contribution to environmental remediation fields and nanocomposite material science.
2 Materials and Methods
Although the electrospinning of PVC and graphene has been investigated in several studies, their combination is still in the early stages of development for oil absorption applications. This represents a novel approach, especially in enhancing and tailoring properties for specific purposes like composite nanosponges designed for oil spill remediation.
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2.1 Materials
A commercial graphene sheet with a thickness of 55 µm and one adhesive side was used for the graphene production. A sodium sulfate solution with a molar mass of 142 g/mol was prepared for electrolysis, ensuring a conductive liquid medium and facilitating ion movement inside the glass container. Polyvinyl chloride (PVC) with a molecular weight (Mw) of 80,000 g/mol was obtained from Sigma-Aldrich (USA). PVC solutions with concentrations of 16 wt% were prepared in a 1:1 (w/w) solvent system of N,N-dimethylformamide (DMF) and tetrahydrofuran (THF). A magnetic stirrer was used to obtain homogeneous solutions.
2.2 Preparation of Graphene Nanoparticles
The synthesis of pristine graphene using a bottom-up approach has proven difficult for industrial applications because of the highly favorable stacking of graphene sheets. Therefore, a top-down approach is more suitable for generating the highly oxidized form of graphene (GO), containing both sp2 and sp3 carbon with abundant oxygen groups [29]. In this method, the electrolysis of graphite involves sending an electric current through an electrolyte solution to stimulate ion flow, facilitating a nonspontaneous reaction, as shown in Fig. 1.
The graphite electrolysis method uses a glass container and two plates as electrodes: one remains stationary while the other is adjustable. A conductive solution was prepared by dissolving sodium sulfate in deionized water. A DC power supply with a voltage range of 10 V was connected to two graphite sheets mounted on plates. The electric current attracts charged ions to the graphite sheets, forcing them between the layers in an intercalation process. With increased heat and energy, the exerted pressure separated the graphite layers into individual parts [30].
After electrolysis, the graphite powder was contaminated with residual salt from the conductive solution, which could be reduced but not eliminated. The graphite particles formed in the solution were filtered and completely dried at 320 °C. After drying, the powder was ground to obtain small particles. A further step was required to reduce the particle size using a water bath sonicator (20–40 kHz, 45 W). The ultrasonic waves exfoliated the graphite layers into smaller sheets. The graphite powder (1.5 g) was added to an ethyl alcohol solution with a concentration of 82.5% v/v (416.75 ml of ethyl alcohol mixed with 88.25 ml of DI water), placed in a sealed glass bottle, and subjected to ultrasonic treatment in a sonic bath for 8 h at 20–40 °C. Glass microfiber filters (Whatman™ GF/A Glass, diameter 3.7 cm, pore size 1.6 µm, thickness 260 µm, weight 53 g/m2) were used to separate the graphene powder. The filtered graphene was dried again in an oven at a low temperature to avoid damage from excessive heat. Figure 2 shows the steps involved in the graphene production from graphite sheets.
Filtered and dried graphene powder was prepared for the XRD analysis. An X-ray diffraction instrument was used to analyze the material’s crystalline structure and identify the crystalline phases present, providing chemical composition information. Scanning was conducted from 2.0° to 35.0° 2θ, with a step size of 0.03° and a dwell time of 0.5 s.
2.2.2 Transmission Electron Microscopy (TEM) Analysis
The graphene particles were examined using transmission electron microscopy (TEM, JEOL Ltd.). Proper specimen preparation is critical for TEM analysis. The sample was dehydrated using alcohol and embedded in plastic, followed by the addition of epoxy plastic to harden it into a solid block. Thin sections were cut using a glass knife. TEM uses transmitted electrons (those passing through the sample) to create an image. Several images of the graphene particles were captured. The average size of the graphene particles was measured for at least 50 particles and the coefficient of variation between the particles was calculated.
2.3 Electrospinning of PVC Nanofibers Loaded with Nanographene
The prepared nanographene powder was dispersed in N,N-dimethylformamide (DMF) solvent using sonication. The nanographene particles (0.5%, 1%, 1.5%, 2% by weight) were mixed with a poly(vinyl chloride) (PVC) aqueous solution using ultrasonic sonication to ensure uniform dispersion of the nanographene in the PVC polymer. The samples of PVC blends containing 0.5–2% nanographene particles were prepared for electrospinning. The electrospinning process consisted of three main components: a syringe with a small-diameter metal spinneret, a high-voltage power supply, and a stationary collector. The graphene/PVC polymer blends were electrospun under constant conditions of 20 kV, a drop height of 20 cm, and a 0.9-mm internal diameter needle [31]. After the samples were fabricated, several tests were conducted to examine the characteristics of both the graphene powder and nanofiber. Figure 2 shows the steps involved in graphene production from graphite sheets and the preparation of PVC/graphene nanoparticles.
2.4 Characterization of Nanofiber Mat
2.4.1 Nanofiber Morphology
The surface morphologies of the composite samples with different graphene ratios were studied using a scanning electron microscope (SEM), JOEL IT 200. Adequately sized nanocomposite samples were carefully cut and mounted onto holders for SEM analysis. The mounted samples were sputter-coated with gold before viewing.
2.4.2 Mechanical Properties of Graphene Nanoparticles/PVC Nanofiber Mat
The tensile strength of the nanofibers with varying graphene ratios was tested using a MesdanLab strength tester equipped with a 100 N load cell, a clamp speed of 50 mm/min, and a gauge length of 40 mm. Five rectangular samples were prepared for each experiment. Each sample was held in two cardboard frames with double-sided adhesive tape to secure the samples. After the nanofiber sample was clamped for testing, the sample holder was cut at the sides using scissors, as shown in Fig. 3.
Fig. 3
Cutting holder after clamping in the tensile tester
The oil spreading in the (x–y) plane was captured on camera as a function of time to apply drop-spreading kinematics. The oil spreading rate of nanofibers with a graphene ratio of 1.5% was investigated. To evaluate the change in the spreading area, the diameters of the oil spills in the x- and y-directions were measured and recorded as a function of time for each sample. A single oil drop weighing 32 mg was released from a droplet tube at a distance of 50 mm. Each experiment was run and recorded at least five times to obtain consistent, dependable data, and to assess the repeatability of the experimental outcomes [32].
3 Results and Discussions
Although the electrospinning of PVC and graphene has been investigated in various studies, their combination remains a developing field, especially regarding commercial applications. This presents a novel approach, particularly in scaling up production and optimizing properties for targeted uses, such as composite nanosponges designed for oil spill cleanup.
3.1 X-ray Diffraction (XRD)
XRD analysis was used to identify unknown substances by comparing their diffraction patterns with those of known materials. The crystalline structures of the synthesized graphite oxide, graphene oxide, and contaminants were analyzed using XRD, as shown in Fig. 4. According to the literature [33], the XRD pattern of graphene shows diffraction peaks at 2θ = 25° and 33°, confirming the successful production of graphene. Improved filtering and washing techniques are required to eliminate contaminants.
The morphological characteristics of the graphene powders were investigated. As shown in Fig. 5, the powder of the created graphene nanoparticles was examined using optical microscopy. Particles with an average size of 34 nm and a coefficient of variation (CV) of 15% were produced. This demonstrates that electrolysis and exfoliation methods were successful in creating graphene nanoparticles.
We conducted an SEM analysis of the produced fibers, as shown in Fig. 6, to investigate the distribution of graphene nanoparticles within the PVC nanofiber matrix. The microstructures and surfaces of the synthesized nanofibers were examined using SEM. Figure 6a–d shows the representative surface morphologies of electrospun PVC nanofibers with different magnifications at 1.0 wt% nanographene particles. SEM analysis revealed solid, uniform nanofibers with random orientations. Compared to pure PVC nanofibers, the average diameter of nanofibers with 1% graphene nanoparticles was 495 nm, with a coefficient of variation (CV) of 32%, resulting in coarser fibers. SEM images in Fig. 6 confirm noticeable differences in the surface morphology of the nanofibers with varying percentages of nanographene particles. These changes in the surface morphology are visible in the SEM images, demonstrating how the addition of nano-graphite to polymer solutions can enhance the mechanical, electrical, and thermal properties of the resulting electrospun nanofibers [34].
SEM images of the nanographene particle/PVC nanofibers show that the graphene nanoparticles are distributed over the surface of the fibers, making the fiber surfaces uneven.
3.4 Mechanical Properties of Electrospun Graphene Particle/PVC Nanofiber Mat
The shape, orientation, and number of fiber contact points within the mat significantly influence its behavior under tension. Mat failure and deformation typically begin with the rupture of inter-fiber junction points [35]. Based on the SEM analysis, no beads were observed, which is beneficial because beads reduce the number of fiber contact points per unit volume in nanofiber mats. More uneven fibers with improved diameter uniformity were formed, increasing the fiber number cohesion points and, consequently, the tensile strength. Electrospun nanofiber mats do not disintegrate into individual fibers; rather, the fiber cohesion points fail [34].
The enhancement in the mechanical tensile properties of the electrospun graphene particle/PVC nanofiber mats is due to the incorporation of graphene particles into the PVC nanofiber matrix. The graphene particles possess high mechanical strength and stiffness, which can improve the mechanical properties of the nanofiber mats. Additionally, the electrospinning process aligns the graphene particles and enhances their dispersion, further contributing to improved mechanical performance [31]. The addition of graphene nanoparticles increased the tensile strength and Young’s modulus depending on the percentage of added nanoparticles. Owing to their high aspect ratio and large surface area, the graphene nanoparticles provide extensive contact area for intermolecular interactions with PVC.
The load–elongation curves of the PVC nanofiber mats and graphene particle/PVC nanofiber mats are shown in Fig. 7. Initially, the elongation increased as the fibers were forced together in the middle of their length, resisting slippage under the applied load. The failure occurred rapidly as the stress levels increased. As illustrated in Fig. 7b, the inclusion of graphene nanoparticles delayed this failure mechanism, allowing the mat to withstand a higher stress before failure.
Fig. 7
Load–elongation curve; a Load–elongation curve for PVC nanofibers. b Load–elongation curve for nanofibers PVC /0.5 nanographene particles
In self-bonded, randomly aligned nanofiber mats, the application of a unidirectional tensile load causes the nanofibers to rotate and align in the direction of the applied force before sliding at the adhesion points between fibers. The load–elongation curve in Fig. 7 explains the breaking mechanism of the randomly aligned nanofiber mats. Two zones are observed on the curve: a high-modulus zone, representing the breaking of adhesion points between fibers under increasing load, and a lower-modulus zone, where fibers slide over each other before total failure [35]. Modifying the surface morphology of the nanofibers increased the surface friction between the fibers, enhancing the breaking strength of the PVC/graphene nanoparticle mat. Fiber sliding under load begins at lower elongation levels.
The tensile strengths were measured for the nanofiber mat with five different percentages of nanographene particles, ranging from 0 to 2 wt%. In each case, the tensile strength reached a maximum and then decreased as the loading of the nanographene particles increased. The highest tensile strength measured was 7.65 MPa, for a 1.5 wt% loading, representing a significant 311% increase in mechanical strength compared to the pure PVC nanofiber mat. This improvement was attributed to the increased fiber cohesion point number, which enhanced the tensile strength. At higher concentrations, it is likely that the nanographene particles agglomerated within the nanofibers and were easily fragmented during the tensile test. Such aggregated nanographene particles would act as structural defects in the nanofibers. The coefficient of variation increased as the percentage of nanographene particles increased [36]. Figure 8 shows the tensile stress of the nanofiber mat with various amounts of nanographene particles.
Fig. 8
The tensile stress of nanofiber mat with varying amounts of nanographene particles
Table 1 presents the sample’s tensile properties with varying percentages of graphene nanoparticles.
Table 1
The Graphene/PVC nanofiber mat tensile properties
Graphene %
Strength MPa
Coefficient of variation(C.V)
Elongation at break %
Young modulus MPa
0
2.46
24.66
12.26
20.07
0.5
6.203
32.24
15.375
40.34
1
6.651
30.07
39.19
16.97
1.5
7.65
61.72
21.56
35.48
2
4.572
66.45
34
13.45
The coefficient of variation (CV%) of tensile strength increases as the percentage of nanographene particles rises, Table 1.
Figure 9 illustrates a typical tensile curve, highlighting five specific points (1–5) observed during tests on five different samples. Point 1 corresponds to zero elongation, while Point 2 marks the initial breaking of fiber bonds. Points 3 and 4 represent the second linear region of the tensile curve and Point 5 indicates fiber breakage [37]. From the analysis of the curves, the bonding between fibers in the nanographene/PVC sample is observed to withstand higher stress compared to the pure PVC mat, resulting in fiber slippage and frictional forces. The slope of the stress–strain curve increases in the second linear region (Points 3–4), while fiber breakage in nanographene-enhanced fibers occurs at higher stress values (Point 5) [37]. From the analysis of the curves, the bonding between fibers in the nanographene/PVC sample is observed to withstand higher stress compared to the pure PVC mat, resulting in fiber slippage and frictional forces. The slope of the stress–strain curve increases in the second linear region (Points 3–4), while fiber breakage in nanographene-enhanced fibers occurs at higher stress values (Point 5).
Fig. 9
Stress–strain curve; a stress–strain curve for PVC nanofibers, b stress–strain curve of 0.5% nanographene particles /PVC nanofibers, c stress–strain curve of 1% nanographene particles /PVC nanofibers
The increase in the CV% of tensile strength with higher nanographene concentrations is attributed to particle agglomeration and clumping, which create inconsistencies and weak points in the fibers. Uneven particle distribution at high concentrations disrupts fiber uniformity and negatively impacts tensile strength [38‐45].
3.5 Application of Nanographene Particles/PVC Mat as an Oil Absorber
The results indicate a significant increase in oil absorption at a graphene concentration of 1.5%. This improvement is attributed to the enhanced surface area and optimized pore graphene nanoparticle structure as shown in Table 2.
Table 2
Change in the oil spill spread shape on the upper surface as a function of time
Key Factors Contributing to Improved Oil Absorption
Larger surface area graphene nanoparticles’ two-dimensional structure provides an extensive surface area, allowing more oil to adhere, enhancing absorption capacity [46, 47].
Figure 10 shows the spreading behavior of oil spills on two sample surfaces. The initial spreading velocity (Vxy) and spread area increase significantly with the incorporation of graphene nanoparticles into PVC nanofibers, resulting in a 20% increase in spread area and a 65% increase in Vxy. This higher Vxy enhances the substrate’s absorption capacity, reducing the oil drop’s lifespan.
Fig. 10
Oil spill spreading area versus time; a PVC nanofibers b PVC nanofibers/1.5% graphene
Nanofibers containing graphene nanoparticles exhibit a more porous structure, facilitating rapid oil absorption immediately after application. As pores fill and absorption capacity diminishes, the spreading rate decreases. The initial high Vxy is driven by surface tension and available surface area. Over time, the contact angle decreases and resistance from the surface slows the spreading rate, as depicted in Fig. 11.
Fig. 11
Spreading velocity of oil spill area versus time for PVC nanofibers and PVC nanofibers/1.5% graphene
This study presents an innovative blend of PVC nanofibers and nanographene particles, an area that remains largely under-researched in prior studies. The use of nanographene to enhance the properties of PVC nanofibers is particularly innovative, with a focus on understanding the effects of varying graphene concentrations.
The research examines the oil absorption potential of PVC nanofibers with graphene particles, showcasing an application that has received limited attention in existing literature. The results demonstrate that a specific graphene concentration (1.5%) significantly improves oil absorption, offering promising implications for environmental cleanup technologies.
The fabrication of PVC nanofibers with graphene nanoparticles represents a cutting-edge approach in nanomaterials, with potential applications in advanced fields such as oil spill remediation. The study reveals that incorporating 1.5% graphene nanoparticles greatly enhances the nanofibers' mechanical and oil absorption properties. At this concentration, Young’s modulus increased from 20.07 ± 14 MPa to 40.34 ± 19 MPa, while tensile strength rose from 2.46 ± 0.2 MPa to 7.65 ± 0.3 MPa. The improved porous structure and expanded surface area of the graphene particles were key factors in boosting oil absorption efficiency and retention capacity.
5 Future Work
Further research should investigate a broader range of nanographene concentrations and particle sizes to optimize the balance between mechanical performance and cost-effectiveness. This would help develop formulations tailored for specific industrial and environmental applications.
Declarations
Conflict of Interest
The authors declare that they have no conflicts of interest.
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