Composites: Part B 58 (2014) 611–617

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Composites: Part B

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Mechanical performance of multiscale basalt fiber–epoxy laminatescontaining tourmaline micro/nano particles

1359-8368/$ - see front matter � 2013 Elsevier Ltd. All rights reserved.http://dx.doi.org/10.1016/j.compositesb.2013.10.034

⇑ Corresponding author at: Division of Mechanical Design Engineering, College ofEngineering, Chonbuk National University, 567 Baekje-daero, Deokjin-gu, Jeonju,Jeonbuk 561-756, Republic of Korea. Tel.: +82 63 270 4763; fax: +82 63 270 2460.

E-mail address: yonjig@jbnu.ac.kr (Y. Kim).

I.D.G. Ary Subagia a,b, Leonard D. Tijing a,c, Yonjig Kim a,d,⇑, Cheol Sang Kim a, Felipe P. Vista IV e,Ho Kyong Shon c

a Division of Mechanical Design Engineering, College of Engineering, Chonbuk National University, 567 Baekje-daero, Deokjin-gu, Jeonju, Jeonbuk 561-756, Republic of Koreab Mechanical Engineering, Faculty of Udayana University, Denpasar, Bali, Indonesiac School of Civil and Environmental Engineering, University of Technology, Sydney (UTS), P.O. Box 123, Broadway, NSW 2007, Australiad Advanced Wind Power System Research Center, Chonbuk National University, Jeonju, Jeonbuk 561-756, Republic of Koreae Department of Electronic Engineering, College of Engineering, Chonbuk National University, 567 Baekje-daero, Deokjin-gu, Jeonju, Jeonbuk 561-756, Republic of Korea

a r t i c l e i n f o a b s t r a c t

Article history:Received 7 November 2012Received in revised form 7 October 2013Accepted 25 October 2013Available online 5 November 2013

Keywords:A. Particle-reinforcementB. Mechanical properties

In this study, the effect of different tourmaline (TM) micro/nano particle loading (i.e., 0.5–2 wt%) on thetensile and flexural properties of a basalt fiber-reinforced epoxy composite laminate (BFRP) was investi-gated. The TM/basalt/epoxy laminates were fabricated by impregnating woven basalt fibers into epoxyresin mixed with TM particles via vacuum assisted resin transfer molding. Tensile and flexural tests wereperformed according to ASTM standards. Fracture surfaces were characterized by scanning electronmicroscopy and energy dispersive spectroscopy. The results showed significant improvement in both ten-sile and flexural strength and modulus when tourmaline particles where incorporated in the basalt/epoxycomposite. The best result was obtained at 1 wt% TM loading with surfactant (i.e., C4) showing anincrease of �16% in both tensile and flexural strength, and 27.4% and 153.3% increase in tensile and flex-ural modulus, respectively, compared to neat basalt/epoxy composite. The enhanced performance of TM/basalt/epoxy laminates is attributed to a good dispersion of TM particles in the epoxy matrix providingincreased surface area for strong interfacial interaction and good load transfer.

� 2013 Elsevier Ltd. All rights reserved.

1. Introduction

Fiber-reinforced polymeric composites (FRCs) are used in manyapplications such as in aerospace, automotive, marine, recreationalequipment, construction, and other high performance applicationsdue to their high stiffness to weight ratio and their ease of process-ing [1,2]. For epoxy-based laminates, fibers such as carbon fiber,glass fiber, and basalt fiber have been used as filler materials to im-prove the overall properties of the composite laminate. Due toenvironmental concerns, recent research has been on the use ofnatural fibers for polymer reinforcement [3]. Flax and hemp fibersare good natural fiber reinforcement materials having acceptablemechanical properties and low cost, however, there is difficultyin maintaining their properties when exposed to high temperature.They are also sensitive to humidity, as well as some experiencingadhesion problem with a polymer matrix [4]. Among the naturalfibers, basalt fiber (BF) has been considered as a potential rein-forcement of composite materials because of the following proper-

ties: good strength, excellent fiber–resin adhesion, soundinsulation properties, low water absorption [5], good resistanceto chemical attack, ecologically friendly, free from carcinogensand health hazards, high operating temperature range, and canbe produced at considerably lower cost than carbon fiber [6–9].Basalt fibers offer an excellent alternative to carbon fibers in differ-ent applications. BF is known to have higher tensile strength thanE-glass fiber and has larger strain-to-failure than carbon fiber [7].The excellent heat resistance and low water absorption of basaltfibers make them suitable as thermal insulation materials andhot fluid conduits [6]. Basalt fibers also showed potential as rein-forcement for concrete mixture, which could provide high fire res-itance. A recent study showed an increase in load-carrying capacityand deflection ductility of timber beams when reinforced with nat-ural fibers including basalt fibers [10]. BFRPs can be utilized in heatshield, thermal insulating barriers and as fire protection [8,11].Moreover, BFRPs showed good potential as an alternative to glassFRP bars for reinforcing concrete structures, especially those struc-tures exposed to repeated load during service such as bridges andparking garages [12]. Additionally, BFRPs can be used as a jacketbonded around concrete columns to enhance their seismic perfor-mance [13]. Thus, BFRPs can potentially replace glass fiber

Fig. 1. Schematic layout of the preparation and fabrication process of the BFRP and composite laminates.

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reinforced polymers for various applications such as in aerospace,construction, transportation, automotive, and shipbuilding.

In recent years, the use of multiple reinforcement length scaleshas been extensively explored in the design of composite lami-nates with improved properties [1,14–17]. Research in nanocom-posites, where micro or nanoparticles (NPs) are incorporated inthe polymeric matrix has generated vast interest in the past twodecades [18]. It opens a new paradigm to tailor the polymer matrixto have optimized properties [19]. Organic or inorganic nanoparti-cles that have high surface-to-volume ratio are used as filler mate-rials, and when incorporated in a polymer matrix can providesynergistic properties that are difficult to obtain separately fromtheir individual components [20,21]. Studies using carbon nano-tubes (CNTs) and carbon nanofibers (CNFs) as fillers in polymercomposites have reported improved mechanical, electrical andthermal properties of the resulting composites [19,22–25]. Bekyar-ova et al. [15] selectively deposited CNTs on woven carbon fabricby electrophoresis, and fabricated a CNT/carbon fabric/epoxy com-posite via a vacuum-assisted resin transfer molding (VARTM) pro-cess. The multiscale composite showed a �30% enhancement ininterlaminar shear strength relative to carbon fiber-reinforce com-posite polymer (CFRP) and demonstrated significantly improvedout-of-plane electrical conductivity. Other reports also indicatedthat surface chemical modification of nanoparticles significantlyhelps in the better dispersion of NPs in the polymeric matrixresulting in enhanced properties of the composite [14,26,27].

Many studies have attempted to enhance the properties of com-posite materials by incorporating nanoclays in the polymeric ma-trix. Inorganic nanoparticles such as nanoclays have gained wideinterest as potential reinforcing materials because of their low costand ease of fabrication [28]. In the present study, nonwoven basaltfiber/epoxy laminates dispersed with 0.5–2.0 wt% tourmaline mi-cro/nanoparticles were fabricated by vacuum assisted resin trans-fer molding (VARTM). Tourmaline (TM) is a polar crystallinematerial belonging to a group of silicate minerals compounded

Table 1Composition and name convention of the laminates used in the present study.

Sample Name conven

Basalt-fiber reinforced plastic (composite) BFRPBasalt/epoxy composite with 0.5 wt% TM (no surfactant) C1Basalt/epoxy composite with 1.0 wt% TM (no surfactant) C2Basalt/epoxy composite with 2.0 wt% TM (no surfactant) C3Basalt/epoxy composite with 1.0 wt% TM (with surfactant) C4

with many elements called cyclosilicates [29,30]. In a previousstudy [31], the incorporation of tourmaline NPs in polyurethanenanofibers increased the mechanical properties of the nanocom-posites. Furthermore, since TM is hydrophilic in nature, the result-ing TM/PU nanofibrous mats showed increased hydrophilicity withthe increase of TM NP content in the nanofiber. Here, we investi-gated the effect of the incorporation of tourmaline micro/nano par-ticles in a basalt fiber-reinforced-epoxy matrix on the mechanicalproperties (i.e., tensile and flexural properties) of the compositelaminates. The fractured surfaces were characterized by scanningelectron microscopy (SEM) and energy dispersive spectroscopy(EDS).

2. Experimental

2.1. Materials

Basalt fiber (EcoB4-F210, woven, 210 ± 10 g/m2) and tourmalinepowder (TM, 325 mesh) were purchased from Seco-Tech, Koreaand UBS Inc., Co., Ltd., Korea, respectively. The size of as-receivedTM particles was about 900 nm–8 lm. The epoxy resin (HTC-667C) and modified aliphatic amine hardener were provided byJet Korea Co., Korea. Acetone (Junsei, Japan) was used to initiallydisperse the TM NPs before mixing with epoxy resin. Triton X-100 was used as a surfactant and was purchased from OCI Com-pany, Ltd., Korea. All chemicals and materials were used asreceived.

2.2. Fabrication of composite laminate

Tourmaline particles were first dispersed in 50 ml acetone byusing a homogenizer operating at 10,000 rpm for 30 min. The highshear force from the homogenizer helps in breaking down theagglomerated TM particles and reduces their size, and properly

tion Concentration of TM particles with respect to epoxy resin (wt%)

00.51.02.01.0 + surfactant

Table 2Summary of the tensile and flexural properties of BFRP and TM particle-reinforced composite laminates.

Sample Tensile properties Flexural properties

Tensile strength(MPa)

% Gain/loss instrength (±)

Modulus(GPa)

% Gain/loss inmodulus (±)

Flexural strength(MPa)

% Gain/loss instrength (±)

Modulus(GPa)

% Gain/loss inmodulus (±)

BFRP 307.5 ± 8.8 0 14.3 ± 0.48 0 229.3 ± 6.0 0 6.5 ± 0.17 0C1 325.7 ± 4.9 +5.9 13.1 ± 1.0 �8.4 232.2 ± 14.8 +1.3 13.6 ± 0.88 +110.1C2 331.0 ± 11.1 +7.6 17.0 ± 0.27 +19.2 239.7 ± 11.8 +4.5 14.7 ± 0.21 +126.9C3 338.9 ± 22.1 +10.2 17.5 ± 0.82 +22.6 252.9 ± 6.3 +10.3 15.4 ± 0.53 +137.7C4 357.2 ± 3.1 +16.1 18.2 ± 0.92 +27.4 266.1 ± 15.8 +16.0 16.4 ± 0.59 +153.3

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disperses the TM particles in the solution. The TM solution wasthen mixed with the epoxy/acetone solution (without hardener)and was stirred overnight. The TM/epoxy/acetone solution was de-gassed in a dry oven at 60 �C for 30 min to evaporate the acetone. Ahardener was then added to the solution and was mixed by manualstirring and then was again degassed for 45 min in a dessicatoryner vacuum to release the trapped bubbles. The concentrationof TM particles was varied from 0.5 wt% to 2 wt% with respect tothe epoxy/hardener solution. Additionally, to check the effect ofsurfactant in the dispersion of TM particles, one sample was pre-pared with Triton X-100 added to the TM/expoxy/acetone solutioncontaining 1 wt% TM particles. The Triton X-100 to TM ratio insolution was 5:1.

Fig. 1 shows a schematic of the preparation and fabrication pro-cess of the present samples. Composite laminates were fabricatedvia a VARTM process. First, 10 layers of basalt fabric with a sizeof 250 mm � 250 mm were stacked in the VARTM stainless steelplate mold (size: 300 mm � 300 mm), and were wrapped with vac-uum bagging film using a sealant tape (AT200Y). The TM/epoxysolution was then injected into the mold through a vacuum pump(�80 kPa) for 30–40 min. The prepared panel (i.e., molded mate-rial) was cured in an autoclave at 65 �C for 2 h. For comparison,neat basalt/epoxy laminate (BFRP) was also prepared as the con-trol. Table 1 shows the composition and name conventions of thesamples prepared in this study.

2.3. Measurements and characterization

Tensile test was performed according to ASTM D 3039M-00 [32]using a universal testing machine (Unitech–M, R&B). The compos-ite plates were cut into dog-bone shape test specimens(L = 165 mm) by water jet cutting. At least five specimens weretested for each sample and the average of which is reported here.The test was conducted at a crosshead speed of 2 mm/min at roomtemperature.

Fig. 2. Typical tensile stress–strain curves of the laminates: (a) BFRP; (b) C1,0.5 wt% TM/basalt/epoxy laminate; (c) C2, 1.0 wt% TM/basalt/epoxy; (d) C3, 2.0 wt%TM/basalt/epoxy, and; (e) C4, 1.0 wt% TM/basalt/epoxy + surfactant. The insetshows the respective optical images of the fractured specimens.

Flexural (three-point bending) test was carried out according toASTM D970 [33]. The average of at least five measurements of eachlaminate sample is reported here. Rectangular shape (L = 76.2 mm,W = 12.7 mm) specimens were used. The crosshead speed wasmaintained at 3 mm/min.

Scanning electron microscopy (SEM, JEOL JSM-5900) was uti-lized to characterize the morphological structure of the tourmalineparticles and the cross-section of the fracture surface of the com-posite laminates. The elements at the cross-section of the sampleswere analyzed by energy dispersive X-ray spectroscopy (EDS) at-tached to SEM machine.

3. Results

Fig. 2 shows typical tensile stress–strain curves of BFRP andcomposite samples. Here, the stress linearly increased withincreasing strain until reaching failure for all samples. BFRP

Fig. 3. Average tensile strength and modulus of the BFRP and TM particle-reinforced composite laminates.

Fig. 4. Average tensile strain of the BFRP and TM particle-reinforced compositelaminates.

Fig. 5. Average flexural strength and modulus of the BFRP and TM particle-reinforced composite laminates.

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showed the lowest tensile strength, while the incorporation of TMparticles has increased the tensile strengths of the composites.Fig. 3 shows the average tensile strength and Young’s modulus ofthe present samples. The basalt/epoxy laminate (i.e., BFRP) showsa tensile strength and modulus of 308 ± 9 MPa and 14 ± 0.5 GPa,

Fig. 6. Representative SEM images of the fracture surfaces after tensile test of: (a) BFRP, (bbasalt fiber) in (d) is shown in (f).

respectively. The incorporation of tourmaline particles in the com-posite laminate showed increasing trend for both tensile strengthand modulus with the increase of TM content. The composite lam-inates showed an increase in tensile strength of 5.9%, 7.6%, 10.2%,and 16.1% for C1, C2, C3, and C4, respectively compared to thatof BFRP (see Table 2). The modulus of elasticity is shown to contin-ually increase with the increase of the TM content. One interestingresult is that with the increase in tensile strength and modulus ofcomposite laminates, there was negligible effect on the tensilestrain of the composites (see Fig. 4). From among the samples,C4, i.e., with the use of surfactant to disperse TM particles, showedthe best results in the improvement of tensile strength and Young’smodulus. The surfactant helped in making the TM particles morehydrophilic, thus improving their dispersibility in the epoxymatrix.

Flexural (3-point) bending tests were performed to check theeffect of TM filler particles on the stiffness and strength of compos-ite laminates. Fig. 5 shows the average flexural strength andYoung’s modulus of the present samples. The flexural strengthsof the composite laminates increased by 1.3%, 4.5%, 10.3%, and16% for C1, C2, C3, and C4, respectively relative to BFRP (see Ta-ble 2). The composite laminates also showed significant improve-ment in the Young’s modulus from bending. The modulus ofBFRP was 6.5 GPa, but when different concentrations of TM parti-cles were loaded, the modulus of composite laminates was

) C1, (c) C2, (d) C3, and (e) C4. The EDS spectra of the boxed area (i.e., TM particle on

Fig. 7. Representative SEM images of the fracture surfaces after flexural test of: (a) BFRP, (b) C1, (c) C2, and (d) C4.

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13.6 GPa, 14.7 GPa, 15.4 GPa, and 16.4 GPa, for C1, C2, C3, and C4,respectively. This translates to an increase of 110–153% in modulusrelative to BFRP. Similar to the results in tensile test, C4 showed thehighest improvement in flexural properties from all the samples.The increased flexural properties signify that TM particles werehomogeneously dispersed in the epoxy matrix.

Fig. 6 shows the SEM images of the fractured surfaces of theBFRP and composite laminates after tensile test. In BFRP (Fig. 6a),a fracture at the resin was observed, with fiber–matrix interfacialdebonding, and separation and fracture of fibers. The compositelaminates with different TM particle contents without surfactant(Fig. 6b–d) showed better fiber–matrix bonding. A few fiber delam-ination in C2 was found. Some TM particle agglomeration could beseen at C3 (Fig. 6d) and voids as well. In C4 (Fig. 6e, i.e., with sur-factant), the fibers were observed to be between the basalt fiber fil-aments and were tightly packed with very good fiber–matrixinterfacial bonding. The EDS spectra (see Fig. 6f) of the boxed areain Fig. 6d confirmed the presence of TM particles on the surface ofbasalt and in the epoxy matrix showing the elemental componentsof TM. Fig. 7 shows the fracture surfaces of the present samplesafter flexural test. BFRP (Fig. 7a) showed some fiber pull-outs andvoids, and fiber–matrix debonding. In C1 (Fig. 7b), some delamina-tion and cracks were seen to occur in the composite. Some brokenfibers are observed in C2 (Fig. 7c), which relates to strong interfa-cial bonding with TM/epoxy matrix, i.e., less fiber pull-outs. A goodepoxy-fiber bonding and well-impregnated TM particles were ob-served in C4 (Fig. 7d).

4. Discussion

The technology in micro/nano particle reinforcement in poly-mer matrix can be categorized into inorganic layered clay technol-ogy, carbon nanotubes (CNTs), carbon nanofibers (CNFs), and metalparticle technology [34–37]. Due to lower cost and ease of fabrica-tion, several inorganic particles have been used for composite rein-forcement such as silica NPs, alumina NPs, boron nitride, andnanoclays to improve the properties of the composite materials[34]. Dean and colleagues [1] reported an increase of 31% and24% in flexural modulus and flexural ultimate strength, respec-tively when they incorporated 2% silicate loading in carbon fiber-

reinforced epoxy laminate. Shahid et al. [38] investigated the effectof chemically-functionalized alumina nanoparticles (carboxylate–alumoxanes) on the performance of CFRP materials. They con-cluded that the miscibility of alumoxane nanoparticle in the resinis of prime importance in the mechanical performance of the com-posite. They also suggested that <5% loadings must be used to pro-vide enhanced performance.

In this study, we used tourmaline micro/nano particles to im-prove the properties of basalt fiber–epoxy composite laminates.To the authors’ best knowledge, no one has reported yet on theuse of tourmaline particles for reinforcement in composite lami-nates. Here, the increase in mechanical properties of compositelaminates is attributed to the efficient stress-transfer from epoxyto TM particles and basalt fibers, originating from the homoge-neous dispersion and the strong interactions between epoxy ma-trix and TM particles, and fiber–epoxy interfacial interaction. Foran effective load transfer of polymer matrix to filler particles, agood dispersion of filler particles is necessary. Studies show thatthe load-transfer mechanism happens due to the mobility of fillerparticles, wherein the particles orient themselves under tensilestress, forming temporary cross-links with polymer matrix, thuscreating a local region of enhanced strength [39]. At high filler con-centration, the TM particles tend to aggregate, which results to lesshomogeneous dispersion in the epoxy matrix, thereby decreasingthe surface area for interfacial adhesion, and decreasing the freevolume for particles to move around [34,40]. The aggregated parti-cles lead to the formation of stress convergence points or as crackinitiation sites [41], thus leading to lower tensile strain [42,43].Especially at the highest TM concentration (C3), clusters of parti-cles were observed (see Fig. 6d), which reflected that some parti-cles agglomerated with each other. This suggests that even afterhigh shear sonication process, the TM particles were not easy todisperse in the epoxy matrix. Similar observation was reportedby Lam et al. [40] using nanoclays subjected to sonication. Basaltfiber is mainly composed of SiO2, Al2O3, CaO, MgO, Fe2O3, TiO2,MnO, and K2O [44]. The structure of basalt fiber is similar to glassfiber, and its main structure is the network structure of –Si–O–Si–[45]. Tourmaline is a silicate-based compound, which also has sim-ilar composition with basalt. In the present study, some of the TMnano-microparticles could have reacted with the silicon hydroxyl

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groups at the basalt fiber surface forming a new –Si–O–Si– bond-ing, which results in more uniform silicon-oxide network structureleading to improve mechanical properties [45]. In this study, theaddition of surfactant (i.e., C4) lead to the better dispersion ofTM particles in the epoxy matrix. This better dispersion providedmore surface area for load transfer of epoxy matrix to TM particles,resulting in increased mechanical properties. Davis et al. [46]attributed the improvement in their composite laminate strengthand stiffness to the enhanced fiber–matrix interfacial strengthdue to fiber–epoxy-f-CNT interfacial covalent bonding.

5. Conclusion

This study investigated the effect of tourmaline micro/nano par-ticle-loading of 0.5–2 wt%, with and without surfactant on themechanical properties of basalt fiber-reinforced epoxy compositelaminate fabricated by a vacuum assisted transfer resin molding.Tensile and flexural tests and fracture surface characterizationswere performed. The composite laminates with different TM load-ings showed improved tensile and flexural properties compared tothe neat basalt fiber–epoxy composite (BFRP). The tensile and flex-ural strengths increased by 5.9–10.2% with negligible effect on ten-sile strain, and 1.3–10.3%, respectively with increasing TM particleloading. The best result was obtained with C4, i.e., at 1 wt% load-ing + surfactant, wherein the tensile and flexural strengths in-creased by 16% and 16.1%, respectively compared to BFRP.Furthermore, the flexural modulus increased by as much as153.3% when loaded with TM particles. SEM images exhibited goodepoxy-fiber bonding and well-impregnated TM particles. Theenhancements in mechanical properties are attributed to the gooddispersion of TM particles in the epoxy matrix, which lead to highsurface area for strong interfacial bonding. This study shows thatthe mechanical properties of neat BFRP can be further enhancedby the homogenous dispersion of TM particles in the epoxy matrix.The good interfacial adhesion between the polymer matrix and ba-salt fibers as well as the effective load transfer from the polymermatrix to the nanoparticles has led to the improvement of themechanical properties. Proper dispersion of micro/nano fillers isan important requisite for effective mechanical property enhance-ment. The expanding applications of BFRPs in industries wouldbenefit from this study and could provide additional informationon the exploitation of micro/nano particles to further enhancethe properties of epoxy-based composite materials.

Acknowledgements

This research was financially supported by the Ministry of Edu-cation, Science and Technology (MEST) and the National ResearchFoundation of Korea (NRF) through the Human Resource TrainingProject for Regional Innovation. I.D.G. Ary Subagia acknowledgesthe support from the Degree General High Education (DGHE) post-graduate abroad scholarship of the Republic of Indonesia for hisPh.D. program at Chonbuk National University in Republic ofKorea.

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