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Improved mechanical properties of graphene-modified basalt fibre–epoxy composites

  • Harun Sepetcioglu , Lubomír Lapčík EMAIL logo , Barbora Lapčíková , Martin Vašina , David Hui , Martin Ovsík , Michal Staněk , Yousef Murtaja , Libor Kvítek , Tereza Lapčíková and Oldřich Zmeškal
Published/Copyright: July 5, 2024
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Nanotechnology Reviews
From the journal Nanotechnology Reviews Volume 13 Issue 1

Abstract

In industrial applications, the potential of basalt fibre-reinforced polymer (BFRP) composite pipes as a compelling alternative to glass and carbon fibre-reinforced composite pipes is recognized. Their high recyclability makes them a viable option for aerospace, marine, and automotive applications. In this study, a comparison is made between the mechanical properties of virgin basalt–epoxy composite pipes and graphene-modified counterparts. To conduct the experiments, pipe section specimens were prepared using a flex grinding machine. Graphene nanoplatelets (GnPs), serving as an exceptional reinforcing material, were uniformly incorporated into the basalt–epoxy composites at a specific concentration. The inclusion of these nanoplatelets resulted in significant changes in mechanical stiffness compared to the virgin basalt–epoxy composite pipes. A series of tests, including uniaxial tensile, Charpy impact, microhardness, Shore D hardness, uniaxial 3-point bending, and dynamic displacement transmissibility tests, were carried out to assess the mechanical properties of both graphene-reinforced and virgin basalt–epoxy pipes. The findings indicated that the pure basalt–epoxy composite exhibited lower ductility compared to the graphene basalt–epoxy composites after undergoing uniaxial mechanical loading. Non-destructive dynamic mechanical vibration testing was used to investigate the complex mechanical response of the materials under examination. The observed complex frequency-dependent responses reflected the mutual ductile/brittle mechanical performance of the developed composites.

Keywords: graphene-modified basalt fibres; composite pipes; epoxy polymer; mechanical testing

1 Introduction

Composite structures are tailored to achieve specific properties suitable for anticipated environments [1,2]. Fibre-reinforced epoxy resin composites have emerged as an advanced material choice for pipe fabrication, surpassing traditional metal pipes in applications such as underground material and fluid transport, including oil, natural gas, wastewater, thermal water, and drinking water. The diverse range of fluids and their associated pressures can significantly impact the material performance. Nevertheless, thanks to their exceptional corrosion resistance, wear resistance, and high strength-to-weight ratio, fibre-reinforced epoxy resin composites offer a substantial advantage over conventional pipe materials [3,4,5,6].

Pressure pulsations, arising from centrifugal pumps or reciprocating compressors in pipeline systems, have well-known detrimental effects on industrial applications. Hydraulic pumps (e.g., centrifugal, piston, or gear pumps), operating on positive displacement principles, inherently produce output flow pulsations leading to pressure pulsations upon encountering liquid resistance. These pulsations traverse the pipeline, causing vibration, noise, damage, and potential safety hazards such as pipes rupture or damage of other components in hydraulic systems [7,8,9,10,11].

Basalt, a natural and environmentally friendly material, is used to produce basalt fibres (BFs) [12]. BFs are more recyclable compared to glass fibres, making them an excellent choice for various applications, including marine, automotive, and aerospace industries where a basalt fibre-reinforced polymer (BFRP) is used [13,14]. They show promise as replacements for glass and carbon fibres due to their exceptional recyclability. BFs have been proven to be non-toxic and non-carcinogenic. These fibres are created by drawing a natural ore through a platinum–rhodium alloy melted at high temperatures [15]. They are cost-effective and possess outstanding properties, including minimal moisture absorption, high-temperature resistance, corrosion resistance, sound absorption, and high strength [16,17,18]. Basalt’s rough surface promotes strong adhesion to the polymer matrix, resulting in robust interfaces. Moreover, BFs exhibit a higher elongation percentage compared to carbon and glass fibres [19].

Epoxy resins serve as the matrix in composite fabrication, offering desirable characteristics such as low shrinkage during curing, excellent heat and chemical resistances, and high strength. However, they have a brittle structure [20,21,22].

Hybrid nanocomposites are typically fabricated by embedding two or more reinforcement materials within the host matrix. This combination enhances specific features, such as ductility, elastic modulus, strength, lightweight properties, and flame retardancy, providing the material with tailored superior properties [23,24,25].

Mechanical and thermal conductivity properties of polymers can be significantly enhanced by introducing carbon-based nano-sized reinforcements, including fullerene [26], carbon nanofibers [27,28], carbon nanotubes [29], and graphene [30].

The discovery of graphene has opened up new avenues for research as it is being incorporated into various composite structures to enhance their properties. Graphene was first isolated and characterized in 2004 by researchers at the University of Manchester (Manchester, UK), using adhesive tape to separate graphite into individual layers of carbon. A decade later, graphene-enhanced composite applications, from aramid nanofiber-reinforced supercapacitors for electric vehicle batteries to aerospace composite tooling and cryogenic pressure vessels, made the headlines. While the material has been commercially available for about a decade, its path to commercialization has significantly accelerated over the past couple of years, with over 2,300 graphene-related patents approved in the last 12 months, according to the Graphene Council (Manchester, UK).

The hexagonally structured single layer of carbon atoms offers extraordinary properties, such as a remarkable thickness of 0.334 nm, a vast specific surface area of approximately 2,600 m2/g, high electron mobility at 200,000 cm²/Vs, thermal conductivity ranging from 3,000 to 5,000 W/mK, exceptional optical transparency at 97.4%, and formidable mechanical strength with a Young’s modulus of elasticity of 1 TPa [31]. These unique properties have opened doors to a diverse range of applications, including energy storage, electronics, healthcare, and construction, with graphene playing a pivotal role in enhancing various material and device performances [32,33,34], e.g., filament-wounded BFRP solid particle erosion property enhancement by the reinforcement of non-functionalized GnPs at a concentration of 0.25% [35].

Graphene nanoplatelets (GnPs) integrated into an epoxy matrix exhibit excellent mechanical properties. The non-isotropic nature of a composite pipe reinforced with GnPs contributes to the enhancement of its mechanical properties, effectively minimizing potential damage from static and variable loads encountered during service conditions [30]. In practical engineering applications, particularly in the design of composite pressure vessels, rocket engine casings in aerospace, transportation of various fluids, safe conveyance and storage of chemicals, marine and offshore structures, penstock applications in hydropower projects, infrastructure projects like bridges and tunnels, cost-effective solutions for agricultural water distribution, and in mining operations for the transport of abrasive materials, the consideration of mechanical loads, both static and variable, holds a paramount significance. The ground-breaking aspect of composite pipes lies in their capacity to amalgamate the robustness of conventional materials with heightened corrosion resistance and prolonged durability. This quality renders GnP-reinforced composite pipes exceptionally well suited for a diverse array of industries and applications [30].

Several studies have been conducted to clarify the influence of GnPs on the mechanical properties of composite structures made from BFs, specifically in plate and pipe configurations. Sepetcioglu et al. [34] investigated the fatigue behaviour of basalt–epoxy composite pressure vessels with the incorporation of GnPs. According to their research, the addition of a small amount of GnPs improved the fatigue life of basalt–epoxy composite pressure vessels [34]. Madhukar and Drzal conducted a study on the low-velocity impact behaviour of twill basalt–epoxy composites by incorporating GnPs. The results indicated that the presence of GnPs in the BEC matrix increases low-velocity impact resistance by reducing absorbed energy during rebound and increasing the contact angle [36]. Bulut investigated the enhancement of interlaminar shear strength, which subsequently improved the flexural and tensile properties through the addition of GnPs to the composite [37]. Boehm explored the mechanical properties of basalt–epoxy composite laminates with the incorporation of GnPs. The findings revealed that adding 0.1 wt% of GnPs to the composite significantly enhanced the bonding strength at the interface, leading to improved mechanical properties [38].

It is well established that graphene is an exceptional material for enhancing composite mechanical properties. In this study, the impact of GnPs incorporated into basalt–epoxy composites on material’s mechanical properties was investigated, with a particular focus on their suitability for pipe applications. The comprehensive mechanical characterization of basalt composite pipes, enhanced with GnPs, is imperative prior to their broad utilization across diverse industries. This necessitates a thorough series of fundamental tests to ascertain their mechanical properties. Therefore, static and dynamic mechanical properties (tensile, bending, micro/nanohardness, unnotched fracture toughness, and vibration damping measurements) of graphene-modified BF–epoxy composite pipes manufactured by the filament winding method were studied. These mechanical tests in an academic context provide a holistic understanding of the composite pipe performance, aiding in material optimization and design for specific industrial needs, ensuring reliability, safety, and longevity.

2 Materials and methods

The unreinforced (Sample 1) and reinforced (Sample 2) BFRP composite pipes (outer diameter of 76 mm and 1 m length) were fabricated using the filament winding technique, as described by Sepetcioglu et al. [34]. The pipe’s wall thickness was of 2 mm. EPIKOTE 828 LVEL bisphenol and EPIKURE 866 hardener agents were chosen as the epoxy resin system (Hexion, Inc., Columbus, Ohio, USA), with monofilament 400 tex BFs measuring 13 μm in diameter (Kamenny Vek, Inc., Dubna, Russian Federation). For epoxy modification, non-functionalized GnPs with a surface area of 800 g/m2, a layer thickness ranging from 3 to 7 nm, an average layer width of 1.5 μm, and a purity of 99.9% were used as nanoreinforcements (Nanografi Nano Technology, Ankara, Turkey). Photographs of cutouts of tested composite pipes are shown in Figure S1. From these pipes, individual testing specimens were prepared for each testing methodology used in this study as described below (Figure 1).

Figure 1 Photograph of cutouts of tested composite pipes.
Figure 1

Photograph of cutouts of tested composite pipes.

To incorporate the GnPs into the polymer matrix, a series of steps were followed. Initially, the GnPs were organized to achieve the desired weight ratio and were then introduced into the pure epoxy resin. The mixture of GnPs and epoxy resin was mechanically stirred for a period of 10–15 min, ensuring the initial dispersion of the GnPs throughout the epoxy matrix. Subsequently, the GnPs and epoxy resin mixture underwent ultrasonic mixing for 30 min to achieve a consistent distribution of GnPs within the epoxy matrix. This ultrasonic process introduced high-frequency sound waves to enhance the uniformity of GnPs, ensuring their even distribution throughout the epoxy [30].

During the winding process, BFs were passed through a drum to allow the impregnation of the GnP/epoxy mixture, ensuring the comprehensive saturation of the BFs with the GnP/epoxy matrix. In this study, a BFRP composite pipe reinforced with 0.25 wt% GnPs (based on our previous experimental optimization) was considered [34].

2.1 Scanning electron microscopy (SEM) analysis

An Axia ChemiSEM scanning electron microscope (Thermo Fisher Scientific, Inc., Seattle, USA) was used for SEM analysis of the fractured surfaces after uniaxial tensile testing. SEM measurements were performed at an accelerating voltage of 2 kV. No coatings of the specimens were used in the experiments.

2.2 Uniaxial tensile testing

A Universal Testing Machine Autograph AGS-100 Shimadzu (Kyoto, Japan) and a Zwick 1456 multipurpose tester (Zwick Roell, Ulm, Germany) equipped with a Compact Thermostatic Chamber TCE Series were used for tensile testing of virgin and graphene-reinforced specimens. All measurements were recorded according to ČSN EN ISO 527-1 and ČSN EN ISO 527-2 standards. Samples were cut by a flex grinding machine GWS 7-125 (Robert Bosch, JSC, Gerlingen, Germany) in dimensions of (25 × 200 × 2) mm (width × length × thickness). These pipe strip specimens, also referred to as pipe section specimens, exhibited curvature on both their inner and outer surfaces [39,40,41]. They were affixed using hydraulic flat jaws. However, it should be mentioned that plastic deformation of the pipe strip specimens at the holding area position can be induced by this clamping procedure. A snapshot photograph of the used uniaxial tensile testing instrument is shown in Figure S2.

Experimental measurements were performed at the room temperature of 25°C with 5 mm/min (Shimadzu instrument) and 10 mm/min (Zwick instrument) strain rates. Young’s modulus of elasticity (E) and the elongation at maximum tensile force (dLmax) were obtained from the stress–strain dependency plots. Each experiment was repeated 10×, and mean values and standard deviations of the measured quantities were subsequently calculated.

2.3 Uniaxial three-point bending tests

The uniaxial three-point bending test was carried out on a Zwick 1456 testing machine (Zwick Roell GmbH &Co. KG, Ulm, Germany) according to the ČSN EN ISO 14125 standard. The results were evaluated using the TestXpert software. The distance between the supports was set to 60 mm, and the roundness of the supports and the load mandrel was 5 mm (Figure 2, scheme of the experimental design). The loading velocity was 50 mm/min. Samples were cut by a flex grinding machine GWS 7-125 (Robert Bosch, JSC, Gerlingen, Germany) in dimensions of (15 × 100 × 2) mm (width × length × thickness). Each measurement was repeated 10×, and mean values and standard deviations of the bending modulus of elasticity (E B), upper yield point (F UY), and elongation at upper yield point (dLFUY) were determined. All experiments were performed at the ambient laboratory temperature of 25°C. A snapshot photograph of the used uniaxial tensile testing instrument in three-point bending test configuration is shown in Figure S3.

Figure 2 Scheme of the experimental setup for three-point bending tests.
Figure 2

Scheme of the experimental setup for three-point bending tests.

2.4 Charpy impact testing

Impact tests were carried out using a Zwick-Roell HIT25P machine (Zwick Roell, Ulm, Germany) according to the ČSN EN ISO 179-2 standard, allowing a 7.5 J energy drop. Samples were cut by a flex grinding machine GWS 7-125 (Robert Bosch, JSC, Gerlingen, Germany) in dimensions of (15 × 50 × 2) mm (width × length × thickness). Each experiment was repeated 10×, and mean values and standard deviations of the fracture toughness (a k) and the absorbed impact work (W) were calculated. All experiments were performed at the ambient laboratory temperature of 25°C.

2.5 Displacement transmissibility measurements

The dynamic mechanical properties of the investigated specimens under harmonic loading were assessed by means of displacement transmissibility, denoted as T d, and defined as follows [42]:

(1) T d = y 2 y 1 = a 2 a 1 .

In this equation, y 1 is the displacement amplitude on the input side of the tested sample, while y 2 is the displacement amplitude on the output side of the tested sample. Similarly, a 1 is the acceleration amplitude on the input side of the tested sample, and a 2 is the acceleration amplitude on the output side of the tested sample. The displacement transmissibility of a spring–mass–damper system, consisting of components such as a spring with stiffness k, a damper with a damping coefficient c, and a mass m, is defined by the following equation [43]:

(2) T d = k 2 + ( c · ω ) 2 ( k − m · ω 2 ) 2 + ( c ∙ ω ) 2 = 1 + ( 2 · ζ · r ) 2 ( 1 − r 2 ) 2 + ( 2 · ζ · r ) 2 .

When the zero value is reached by the derivative dT d/dr in equation (2), the frequency ratio r 0 at which the maximum value of displacement transmissibility is attained can be determined [44,45]:

(3) r 0 = 1 + 8 · ζ 2 − 1 2 · ζ .

Equation (3) clearly demonstrates that as the damping ratio ζ increases, or as the material’s mechanical stiffness k decreases, the local extreme of the displacement transmissibility tends to shift towards lower frequency ratios r.

To conduct mechanical vibration tests, the forced oscillation method was applied. The displacement transmissibility, T d, was quantified through experimental measurements. This was accomplished using a BK 4810 vibrator, in conjunction with a BK 3560-B-030 signal pulse multi-analyser and a BK 2706 power amplifier, spanning a frequency range from 2 to 1,600 Hz. The input and output sides of the test specimens were equipped with BK 4393 accelerometers (Brüel & Kjær, Nærum, Denmark) to record acceleration amplitudes a 1 and a 2.

The measurements of displacement transmissibility were conducted on test samples of the following dimensions: 15 mm in width, 60 mm in length, and 2 mm in thickness. These tests involved two inertial masses (m i) weighing 90 and 300 g, respectively, placed on the top side of the tested specimens. Each measurement was repeated 10×, all conducted under ambient conditions at a temperature of 25°C.

2.6 Micro-hardness testing

Micro-indentation tests were performed on a micro-indentation tester (Micro Combi Tester, Anton Paar, Graz, Austria) according to the ČSN EN ISO 14577 standard. The applied diamond tip was cube-corner-shaped (Vickers, Anton Paar, Graz, Austria). Measurement parameters were set as follows: a maximum load of 3 N, a loading rate (unloading rate) of 6 N/min, and a holding time of 90 s. Samples were cut by a flex grinding machine GWS 7-125 (Robert Bosch, JSC, Gerlingen, Germany) in dimensions of (15 × 100 × 2) mm (width × length × thickness). All experiments were performed according to the depth sensing indentation method, allowing simultaneous measurement of the acting force on the indenter and the displacement of the indenter’s tip. The embossing modulus (E IT) was calculated from the plane strain modulus of elasticity (E*) using an estimated Poisson’s ratio (ν) of 0.35 for the studied samples [35,46]:

(4) E IT = E * ( 1 − ν 2 )

The indentation hardness (H IT) was measured as well. Each measurement was repeated 10×, and mean values and standard deviations of the indentation modulus were calculated. All experiments were performed at the ambient laboratory temperature of 25°C.

2.7 Shore D hardness measurements

Shore D hardness measurements were performed on an AFFRI Microhardness DM2D instrument (AFFRI, Inc., Wood Dale, IL, USA). The holding time was set to 4 s, and the applied method was “Shore D.” Samples were cut by a flex grinding machine GWS 7-125 (Robert Bosch, JSC, Gerlingen, Germany) in dimensions of (15 × 100 × 2) mm (width × length × thickness). Each measurement was repeated 10×, and mean values and standard deviations of Shore D hardness were calculated. All experiments were performed at the ambient laboratory temperature of 25°C.

2.8 Statistical analysis

All experiments were repeated 10×. Experimental results were expressed as average values with standard deviations. SigmaPlot 12.5 software (Systat Software, Inc., San Jose, CA, USA) was used for the statistical analysis of data, and significance was determined through one-way analysis of variance (ANOVA) with a significance level set at p < 0.05. The normality of data distributions was confirmed using Shapiro–Wilk normality tests.

3 Results and discussion

3.1 SEM analysis and uniaxial tensile testing

Figure 3 depicts typical stress–strain patterns for the tested Samples 1 and 2 at a deformation rate of 5 mm/min. Three distinct deformation regions were clearly distinguished. The initial region corresponded to the linear elastic phase, typically observed for relative strains less than 0.02. An increase of 5% in the upper yield strain was observed for the GnP-reinforced composite compared to the virgin basalt epoxy specimen. However, this phase was characterized by the brittle fracture of both the epoxy matrix and the BF bundles, as confirmed by SEM analysis (Figure 3a inset).

Figure 3 Results of the uniaxial tensile testing of studied materials at the 5 mm/min deformation rate: red line – sample 1, black line – sample 2. Insets: SEM images of the fracture surfaces of the tested samples (a – 80× magnification, b – 30× magnification).
Figure 3

Results of the uniaxial tensile testing of studied materials at the 5 mm/min deformation rate: red line – sample 1, black line – sample 2. Insets: SEM images of the fracture surfaces of the tested samples (a – 80× magnification, b – 30× magnification).

Following the elastic region, a subsequent plastic deformation phase occurred, marked by the matrix’s elongation and simultaneous frictional sliding of the fibres. This phase took place at relative strains ranging from 0.02 to 0.03.

Finally, a third debonding region was observed, where individual BF bundles were pulled out from the epoxy matrix, ultimately leading to specimen fracture (Figure 3b inset, SEM of the fracture surface). The step-like stress–strain pattern observed was attributed to the ongoing process of individual BF debonding.

Notably, in the low-strain elastic region, two consecutive linear elastic behaviour patterns were observed, as depicted in Figure 4. These patterns were modelled as the linear dependencies of the stress, represented as stress = b[1] × strain + b[0]. The observed Young’s modulus of elasticity, denoted as b[1], was found to be 7.84 GPa for virgin basalt-epoxy composites (Sample 1). However, in the case of graphene-modified matrices (Sample 2), the observed Young’s modulus of elasticity increased to 8.67 GPa for lower strains. Conversely, for higher strains ranging from 0.004 to 0.016, a decreased Young’s modulus of elasticity of 4.57 GPa was noted.

Figure 4 Details of the stress–strain dependencies of the studied materials observed at a 5 mm/min deformation rate. Inset: Parameters of the linear regression fittings of the tangents of the linear elastic parts: b[1] – Young’s modulus of elasticity; b[0] – initial residual bias: (a) – sample 1, (b) – sample 2.
Figure 4

Details of the stress–strain dependencies of the studied materials observed at a 5 mm/min deformation rate. Inset: Parameters of the linear regression fittings of the tangents of the linear elastic parts: b[1] – Young’s modulus of elasticity; b[0] – initial residual bias: (a) – sample 1, (b) – sample 2.

Based on these findings, it can be concluded that the first steeper tangent represents the Young’s modulus of elasticity (E) of BFs, while the second tangent represents the E of the epoxy matrix, in alignment with the findings of Khalid et al. [47]. The obtained intercept magnitudes, b[0], in the first elastic region were 1.39 MPa for Sample 1 and 0.65 MPa for Sample 2. These values indicated a slippage-induced bias dissipation mechanism in the graphene-modified specimens. This interpretation was based on the assumption that it follows a similar fashion to the case of the initial residual bias, which occurs due to pre-existing stress in samples resulting from the process of stretching and extending of the fabric material at an angle or direction not aligned with the primary warp and weft directions of the fabric [48].

Results of the uniaxial tensile testing at 10 mm/min deformation rate are shown in Figure 5 and Table 1. Young’s modulus of elasticity (E) was increased to 11.25 GPa for Sample 1 and to 10.44 GPa for Sample 2 compared to the elastic moduli obtained for the 5 mm/min deformation rate. This confirmed a more rigid response of the matrix to the applied loads for measurements at 10 mm/min deformation rate. The obtained deformations at maximum force were higher in the case of Sample 2 (1.92%) compared to Sample 1 (1.88%). This was assumed to be due to the successful frictional sliding of GnPs proceeding within the complex composite matrix similar to that observed in carbon nanotubes’ epoxy honeycomb sandwich panel composites [29].

Figure 5 Results of uniaxial tensile testing for the studied samples at a deformation rate of 10 mm/min. (a) Young’s modulus of elasticity. (b) Elongation at maximum tensile force. Box plot parameters: Long dashed lines indicate mean values, solid lines represent median values, and corresponding outliers. Obtained mean and median values of both parameters were not statistically significantly different as determined through one-way ANOVA (p > 0.05). Data match the pattern expected if the data were drawn from a population with a normal distribution as obtained by the Shapiro–Wilk normality test.
Figure 5

Results of uniaxial tensile testing for the studied samples at a deformation rate of 10 mm/min. (a) Young’s modulus of elasticity. (b) Elongation at maximum tensile force. Box plot parameters: Long dashed lines indicate mean values, solid lines represent median values, and corresponding outliers. Obtained mean and median values of both parameters were not statistically significantly different as determined through one-way ANOVA (p > 0.05). Data match the pattern expected if the data were drawn from a population with a normal distribution as obtained by the Shapiro–Wilk normality test.

Table 1

Summary of the results of the measured quantities of the studied composite samples

Parameter Sample 1 Sample 2
E (GPa) 11.25 ± 1.22a 10.44 ± 1.45a
dLmax (%) 1.88 ± 0.17a 1.92 ± 0.21a
E B (GPa) 12.86 ± 0.78a 13.09 ± 0.57a
dLUY (mm) 14.02 ± 1.32a 14.23 ± 1.52a
F UY (N) 125.60 ± 9.05a 134.90 ± 7.22b
a K (J/m2) 125.19 ± 15.62a 164.03 ± 20.81b
W (J) 4.01 ± 0.50a 5.25 ± 0.67b
f R1 (m i = 90 g) (Hz) 653.38 ± 21.25a 706.42 ± 20.19b
f R1 (m i = 300 g) (Hz) 305.66 ± 10.12a 411.37 ± 13.31b
E IT (GPa) 4.44 ± 0.09a 4.25 ± 0.06b
H IT (MPa) 225.15 ± 7.12a 211.16 ± 3.52b
Shore D (−) 88.87 ± 1.67a 86.25 ± 2.34b

Differences in the mean values among the statistical groups were tested at a significance level of p < 0.05. The Tukey test was applied for multiple comparisons of the mean values to assess the statistical significance, i.e., to evaluate if the differences were greater than what would be expected by chance; different superscript letters were used to indicate statistically significant differences between the values determined. The results were expressed as arithmetic mean ± standard deviation.

3.2 Uniaxial three-point bending tests

The results of uniaxial three-point bending tests are presented in Figures 6 and 7. The observed bending modulus of elasticity increased from 12.86 GPa for Sample 1 to 13.09 GPa after the addition of planar GnPs into the composite structure (Figure 6a). This increase indicated a greater bending stiffness when subjected to perpendicular loading acting via the specimen’s cross-section.

Figure 6 Results of uniaxial three-point bending tests for the studied composites (at a deformation rate of 50 mm/min). (a) Bending modulus of elasticity. (b) Elongation at the yield point. Box plot parameters: Long dashed lines indicate mean values, solid lines represent median values, and corresponding outliers. Obtained mean and median values of both parameters were not statistically significantly different as determined through one-way ANOVA (p > 0.05). Data match the pattern expected if the data were drawn from a population with a normal distribution as obtained by the Shapiro–Wilk normality test.
Figure 6

Results of uniaxial three-point bending tests for the studied composites (at a deformation rate of 50 mm/min). (a) Bending modulus of elasticity. (b) Elongation at the yield point. Box plot parameters: Long dashed lines indicate mean values, solid lines represent median values, and corresponding outliers. Obtained mean and median values of both parameters were not statistically significantly different as determined through one-way ANOVA (p > 0.05). Data match the pattern expected if the data were drawn from a population with a normal distribution as obtained by the Shapiro–Wilk normality test.

Figure 7 Force at the yield point obtained by the uniaxial three-point bending test of the studied composites. Box plot parameters: Long dashed lines indicate mean values, solid lines represent median values, and corresponding outliers. Obtained mean and median values of both parameters were statistically significantly different as determined through one-way ANOVA (p < 0.05). Data match the pattern expected if the data were drawn from a population with a normal distribution as obtained by the Shapiro–Wilk normality test.
Figure 7

Force at the yield point obtained by the uniaxial three-point bending test of the studied composites. Box plot parameters: Long dashed lines indicate mean values, solid lines represent median values, and corresponding outliers. Obtained mean and median values of both parameters were statistically significantly different as determined through one-way ANOVA (p < 0.05). Data match the pattern expected if the data were drawn from a population with a normal distribution as obtained by the Shapiro–Wilk normality test.

These effects were also reflected in the observed elongations at upper yield points (Figure 6b), which increased from 14.02 mm (Sample 1) to 14.23 mm (Sample 2). Analogous to the previously discussed uniaxial tensile tests, it was proposed that this behaviour provided clear evidence of the continuous frictional sliding of the flat phases of the GnPs within the composite matrix. The hypothesized energy-dissipative pathways, relying on the latter-mentioned frictional sliding of GnPs and the simultaneous debonding and pull-out of BFs, were further substantiated by the increased forces observed at the upper yield points, increasing from 125.6 N (Sample 1) to 134.9 N (Sample 2), as illustrated in Figure 7 and detailed in Table 1.

3.3 Fracture toughness measurements

The results of fracture toughness measurements for the studied composites are presented in Figure 8 and Table 1. It is recognized that achieving high mechanical toughness in a material necessitates not only sufficient high material strength but also adequate deformability. The energy required to fracture the test specimen encompasses multiple components. In addition to the generation of new fracture surfaces, a significant portion of the hammer’s energy is expended on viscoelastic or plastic deformations within the material surrounding the fracture surface or on the bending deformation of the entire test specimen. Another energy portion is converted into the kinetic energy of flying fragments or acoustic emissions or is absorbed by the testing equipment [49]. It was found that the graphene-reinforced Sample 2 exhibited an approximate 31% increase in fracture toughness (a k = 164.03 J/m²) compared to the unmodified Sample 1 (a k = 125.17 J/m²). A similar trend was also observed for the absorbed impact work, with a 31% increase as well (W = 5.25 J for Sample 2 and W = 4.01 J for Sample 1).

Figure 8 Results of Charpy pendulum impact tests for the studied composites. (a) Fracture toughness. (b) Absorbed impact work. Box plot parameters: Long dashed lines indicate mean values, solid lines represent median values, and corresponding outliers. Obtained mean and median values of both parameters were statistically significantly different as determined through one-way ANOVA (p < 0.05). Data match the pattern expected if the data were drawn from a population with a normal distribution as obtained by the Shapiro–Wilk normality test.
Figure 8

Results of Charpy pendulum impact tests for the studied composites. (a) Fracture toughness. (b) Absorbed impact work. Box plot parameters: Long dashed lines indicate mean values, solid lines represent median values, and corresponding outliers. Obtained mean and median values of both parameters were statistically significantly different as determined through one-way ANOVA (p < 0.05). Data match the pattern expected if the data were drawn from a population with a normal distribution as obtained by the Shapiro–Wilk normality test.

3.4 Vibration-excited dynamic mechanical testing

The results of the vibration-excited dynamic mechanical tests of the studied composite pipe’s specimens are shown in Figure 9 and summarized in Table 1. The obtained frequency dependencies revealed distinct first resonant peak frequencies (f R1) in the displacement transmissibility, reflecting the materials mechanical stiffness of the tested composites. It was observed in excellent agreement with equation (3) that higher f R1 values corresponded to the higher mechanical stiffness of the composite matrix [42,43]. Figure 9 illustrates that Sample 2 (with a GnP-modified matrix) consistently exhibited higher f R1 values, regardless of the applied inertial mass, compared to Sample 1 (with an unmodified composite matrix). This indicated that the addition of GnPs increased the mechanical stiffness of the composite matrix, making it suitable for applications in pipes subjected to high-pulsatile hydraulic pressure. A similar reinforcement effect was found for carbonaceous fillers in epoxy resin composites as well [29]. Therefore, these novel composites are excellent candidates for use in critical infrastructure or high-loaded pressurized components of tubular transport systems. Additionally, the increased mechanical stiffness of the GnP-reinforced composites led to higher durability [34], low weight, and simultaneous anticorrosive properties. The observed dynamic mechanical behaviour aligned positively with fracture toughness measurements, where the fracture toughness (a k) increased when graphene was incorporated into the composite matrix structure.

Figure 9 Frequency dependencies of the displacement transmissibility for the tested composites with applied inertial masses of 90 and 300 g.
Figure 9

Frequency dependencies of the displacement transmissibility for the tested composites with applied inertial masses of 90 and 300 g.

Furthermore, a shift in f R1 towards lower excitation frequencies was observed with increasing inertial mass pre-loading of the specimen during dynamic mechanical vibrator testing. Because the natural frequency of the undamped system is proportional to the square root of the ratio of the material stiffness to the applied inertial mass [50], this leads to a decreasing dependence of the first resonance frequency with increasing inertial mass for each of the studied composites, as shown in Figure 9. This shift signifies that as the inertial mass increases, the system’s tendency to vibrate at lower frequencies becomes more prominent. This effect plays a crucial role in energy damping mechanisms for vibration isolation. The lower frequency f R1 of the composite system at higher inertial mass suggests that the system is less inclined to vibrate at higher frequencies, resulting in increased stability. This trend is evident from Eq. (3), which shows that the local extreme of the displacement transmissibility generally shifts to lower values of the frequency ratio (r) as the damping ratio (ζ) increases or as the material stiffness (k) decreases.

3.5 Micro-hardness and Shore D hardness testing

The results of microhardness tests shown in Figure 10 confirmed the decrease of the measured indentation modulus (E IT) after incorporation of the GnP filler into the composite matrix. E IT decreased from 4.44 GPa (Sample 1) to 4.25 GPa (Sample 2). This behaviour was attributed to the plasticizing effect induced by the incorporated nanofillers within the composite matrix. These filler particles impacted the surface layers of the testing specimens. This assumption was further supported by the reduction in microhardness (H IT), which decreased from 225.15 MPa (Sample 1) to 211.16 MPa (Sample 2). The obtained Shore D hardness of 86.25 of the graphene-modified Sample 2 was lower compared to the unmodified Sample 1 hardness of 88.87. This lower Shore D hardness reflected the same plasticizing effect of GnPs in the complex composite matrix as that observed in the microhardness measurements discussed above (Table 1).

Figure 10 Results of micro-hardness measurements of the studied composites: (a) Embossing modulus (E IT). (b) Indentation hardness (H IT).
Figure 10

Results of micro-hardness measurements of the studied composites: (a) Embossing modulus (E IT). (b) Indentation hardness (H IT).

4 Conclusions

In this study, the increase in mechanical stiffness of basalt–epoxy composite pipes after incorporation of GnPs into the epoxy matrix was confirmed. An extensive set of experimental tests included uniaxial tensile tests, uniaxial three-point bending tests, fracture toughness measurements, vibration-induced dynamic mechanical tests, microhardness, and Shore hardness tests. The microstructure of the fracture surfaces was analysed by means of SEM. The simultaneous combination of fracture mechanisms initiated by the applied mechanical load, including the brittle fracture of the epoxy matrix, ductile fracture mechanisms such as BF separation, and internal friction of the GnPs, was confirmed. The results demonstrated changed material’s mechanical properties, including Young’s modulus of elasticity, elongation at break, hardness, mechanical stiffness and toughness, resulting from the incorporation of GnPs into the complex composite matrix. These changes were accompanied by observed plasticization effects, resulting in an approximate 2% increase in mechanical bending stiffness and a significant rise in fracture toughness from 125 to 164 J/m² (approximately 31%) in the composite tubular matrix. Additionally, there was an observed increase in dynamic mechanical stiffness from vibration damping tests of the GnP-modified epoxy composite pipe, making it suitable for a wide range of applications subjected to high-pulsatile hydraulic pressure. Therefore, these novel GnP-basalt–epoxy composites are excellent candidates for critical infrastructure or high-loaded pressurized tubular transport components.

Acknowledgments

MV expresses his gratitude for the financial support of this research through Project No. CZ.02.01.01/00/22_008/0004631 and “Materials and Technologies for Sustainable Development,” within the Jan Amos Komensky Operational Program, funded by the European Union and the state budget of the Czech Republic. LL, BL, LK, and YM would like to extend their thanks for the funding provided by the Internal Grant of Palacky University in Olomouc (IGA_PrF_2023_024 and IGA_PrF_2024_020). Special thanks also due to Aleš Panáček (Palacky University Olomouc) for conducting SEM measurements.

  1. Funding information: This research was funded by the project No. CZ.02.01.01/00/22_008/0004631, “Materials and Technologies for Sustainable Development,” within the Jan Amos Komensky Operational Program, funded by the European Union and the state budget of the Czech Republic as well as by the Internal Grant of Palacky University in Olomouc (IGA_PrF_2023_024 and IGA_PrF_2024_020).

  2. Author contributions: All authors have accepted responsibility for the entire content of this manuscript and approved its submission.

  3. Conflict of interest: David Hui, who is the co-author of this article, is a current Editorial Board member of Nanotechnology Reviews. This fact did not affect the peer-review process. The authors declare no other conflict of interest.

  4. Data Availability Statement: The data presented in this study are available on Zenodo 2022 https://zenodo.org/records/10819340 [55].

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Received: 2023-11-10
Revised: 2024-04-09
Accepted: 2024-06-11
Published Online: 2024-07-05

© 2024 the author(s), published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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  119. A comprehensive systematic literature review of ML in nanotechnology for sustainable development
  120. Exploiting the nanotechnological approaches for traditional Chinese medicine in childhood rhinitis: A review of future perspectives
  121. Twisto-photonics in two-dimensional materials: A comprehensive review
  122. Current advances of anticancer drugs based on solubilization technology
  123. Recent process of using nanoparticles in the T cell-based immunometabolic therapy
  124. Future prospects of gold nanoclusters in hydrogen storage systems and sustainable environmental treatment applications
  125. Preparation, types, and applications of one- and two-dimensional nanochannels and their transport properties for water and ions
  126. Microstructural, mechanical, and corrosion characteristics of Mg–Gd–x systems: A review of recent advancements
  127. Functionalized nanostructures and targeted delivery systems with a focus on plant-derived natural agents for COVID-19 therapy: A review and outlook
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  135. Graphitic carbon nitride hybrid thin films for energy conversion: A mini-review on defect activation with different materials
  136. Nanoparticles and the treatment of hepatocellular carcinoma
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  139. Recent progress in nanomaterials of battery energy storage: A patent landscape analysis, technology updates, and future prospects
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  153. An environmentally greener and reusability approach for bioenergy production using Mallotus philippensis (Kamala) seed oil feedstock via phytonanotechnology
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  164. Poly-3,4-dihydroxybenzylidenhydrazine, a different analogue of polydopamine
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  166. Advancing resource sustainability with green photothermal materials: Insights from organic waste-derived and bioderived sources
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  174. Metal oxides on the frontlines: Antimicrobial activity in plant-derived biometallic nanoparticles
  175. Controlling pore size during the synthesis of hydroxyapatite nanoparticles using CTAB by the sol–gel hydrothermal method and their biological activities
  176. Special Issue on State-of-Art Advanced Nanotechnology for Healthcare
  177. Applications of nanomedicine-integrated phototherapeutic agents in cancer theranostics: A comprehensive review of the current state of research
  178. Smart bionanomaterials for treatment and diagnosis of inflammatory bowel disease
  179. Beyond conventional therapy: Synthesis of multifunctional nanoparticles for rheumatoid arthritis therapy
https://doi.org/10.1515/ntrev-2024-0052
Keywords for this article
graphene-modified basalt fibres; composite pipes; epoxy polymer; mechanical testing
Creative Commons
BY 4.0

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  137. Special Issue on Advanced Nanomaterials and Composites for Energy Conversion and Storage - Part II
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  146. Incorporating GO in PI matrix to advance nanocomposite coating: An enhancing strategy to prevent corrosion
  147. Synthesis, characterization, thermal stability, and application of microporous hyper cross-linked polyphosphazenes with naphthylamine group for CO2 uptake
  148. Engineering in ceramic albite morphology by the addition of additives: Carbon nanotubes and graphene oxide for energy applications
  149. Nanoscale synergy: Optimizing energy storage with SnO2 quantum dots on ZnO hexagonal prisms for advanced supercapacitors
  150. Aging assessment of silicone rubber materials under corona discharge accompanied by humidity and UV radiation
  151. Tuning structural and electrical properties of Co-precipitated and Cu-incorporated nickel ferrite for energy applications
  152. Sodium alginate-supported AgSr nanoparticles for catalytic degradation of malachite green and methyl orange in aqueous medium
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  154. Micro-/nano-alumina trihydrate and -magnesium hydroxide fillers in RTV-SR composites under electrical and environmental stresses
  155. Mechanism exploration of ion-implanted epoxy on surface trap distribution: An approach to augment the vacuum flashover voltages
  156. Nanoscale engineering of semiconductor photocatalysts boosting charge separation for solar-driven H2 production: Recent advances and future perspective
  157. Excellent catalytic performance over reduced graphene-boosted novel nanoparticles for oxidative desulfurization of fuel oil
  158. Special Issue on Advances in Nanotechnology for Agriculture
  159. Deciphering the synergistic potential of mycogenic zinc oxide nanoparticles and bio-slurry formulation on phenology and physiology of Vigna radiata
  160. Nanomaterials: Cross-disciplinary applications in ornamental plants
  161. Special Issue on Catechol Based Nano and Microstructures
  162. Polydopamine films: Versatile but interface-dependent coatings
  163. In vitro anticancer activity of melanin-like nanoparticles for multimodal therapy of glioblastoma
  164. Poly-3,4-dihydroxybenzylidenhydrazine, a different analogue of polydopamine
  165. Chirality and self-assembly of structures derived from optically active 1,2-diaminocyclohexane and catecholamines
  166. Advancing resource sustainability with green photothermal materials: Insights from organic waste-derived and bioderived sources
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  168. Special Issue on Implementing Nanotechnology for Smart Healthcare System
  169. Intelligent explainable optical sensing on Internet of nanorobots for disease detection
  170. Special Issue on Green Mono, Bi and Tri Metallic Nanoparticles for Biological and Environmental Applications
  171. Tracking success of interaction of green-synthesized Carbopol nanoemulgel (neomycin-decorated Ag/ZnO nanocomposite) with wound-based MDR bacteria
  172. Green synthesis of copper oxide nanoparticles using genus Inula and evaluation of biological therapeutics and environmental applications
  173. Biogenic fabrication and multifunctional therapeutic applications of silver nanoparticles synthesized from rose petal extract
  174. Metal oxides on the frontlines: Antimicrobial activity in plant-derived biometallic nanoparticles
  175. Controlling pore size during the synthesis of hydroxyapatite nanoparticles using CTAB by the sol–gel hydrothermal method and their biological activities
  176. Special Issue on State-of-Art Advanced Nanotechnology for Healthcare
  177. Applications of nanomedicine-integrated phototherapeutic agents in cancer theranostics: A comprehensive review of the current state of research
  178. Smart bionanomaterials for treatment and diagnosis of inflammatory bowel disease
  179. Beyond conventional therapy: Synthesis of multifunctional nanoparticles for rheumatoid arthritis therapy
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