investigation of the effect of surface modifications on the mechanical properties of basalt fibre...

Composites: Part B 43 (2012) 812–818

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Composites: Part B

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Investigation of the effect of surface modifications on the mechanical propertiesof basalt fibre reinforced polymer composites

V. Manikandan, J.T. Winowlin Jappes ⇑, S.M. Suresh Kumar, P. AmuthakkannanDepartment of Mechanical Engineering, Kalasalingam University, Krishnankoil 626 190, Tamilnadu, India

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

Article history:Received 10 June 2010Received in revised form 16 August 2011Accepted 1 November 2011Available online 13 November 2011

Keywords:A. FibresB. Mechanical propertiesD. FractographyE. Surface treatments

1359-8368/$ - see front matter � 2011 Elsevier Ltd. Adoi:10.1016/j.compositesb.2011.11.009

⇑ Corresponding author.E-mail address: [email protected] (J.T. Winow

Unsaturated polyester-based polymer composites were developed by reinforcing basalt fabric into anunsaturated polyester matrix using the hand layup technique at room temperature. This study describesbasalt fibre reinforced unsaturated polyester composites both with and without acid and alkali treat-ments of the fabrics. The objective of this investigation was to study the effect of surface modifications(NaOH & H2SO4) on mechanical properties, including tensile, shear and impact strengths. Variations inmechanical properties such as the tensile strength, the inter-laminar shear strength and the impactstrength of various specimens were calculated using a computer-assisted universal testing machineand an Izod Impact testing machine. Scanning Electron Microscope (SEM) observations of the fracturesurface of the composites showed surface modifications to the fibre and improved fibre–matrix adhesion.The result of the investigation shows that the mechanical properties of basalt fibre reinforced compositesare superior to glass fibre reinforced composites. This work confirms the applicability of basalt fibre as areinforcing agent in polymer composites.

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1. Introduction

Natural fibres are now considered as a serious alternative toglass fibres for use in composite materials as reinforcing agents.The advantages of natural fibres over glass fibres are their low cost,low density, high strength-to-weight ratio, resistance to breakageduring processing, low energy content and recyclability [1]. Sincethey are waste, the utilization of natural fibres as reinforcementfor polyester composite is a best eco-reusing technique [2]. Naturalfibres can be divided into two groups: natural fibres, which areavailable in a fibre form, and fibres with a natural origin that areartificially produced from natural raw materials. Currently, glass fi-bre is the typical reinforcing material for polymer composites. Car-bon fibre is used when there are more specialised and greaterrequirements (e.g., space technology, the aircraft industry, militaryapplications and sports). However, carbon fibre’s production costsare one order of magnitude greater than those of glass fibre, andadhesion between carbon fibres and the matrix is also more diffi-cult to achieve [3]. Natural fibres like flax, sisal, coir, hemp, etc.are becoming more popular because it has satisfactory strengthproperties along with a relatively low price and good biodegrad-ability. A disadvantage of these fibres is that the consistency ofthe fibres cannot be guaranteed; they are sensitive to the moisturecontent of the environment, and they do not adhere well to a poly-

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lin Jappes).

mer matrix under moist conditions [4]. Considering that the fibremarket is very competitive and that the economic and environmen-tal requirements imposed on plastic structural reinforcing elementsare increasing, the applicability of newer fibres is being examined inleading research institutes throughout the world. Basalt fibreswhich extracted from common volcanic rock could be a good optionfor reinforcing with polymer matrices [5]. Its chemical compositionis closely similar to glass; its basic components are SiO2, Al2O3, CaO,MgO, K2O, Na2O, Fe2O3 and FeO [6]. Thus, over the last few years,intensive research has begun on the applicability of basalt fibre asa reinforcing material for polymers. Its melting temperature rangesbetween 1350 and 1700 �C. When cooled slowly, basalt solidifies asa partially crystalline structure. Basalt fibres can be used from 200to 600 �C without any significant loss of mechanical properties[7,8]. To enhance fracture toughness, basalt fibres were introducedinto concrete composites by Dias and Thaumaturgo [9]. Sim inves-tigated the durability and mechanical properties of basalt fibresstrengthening structural concrete [10]. Studies on the use of basaltfibres as reinforcements of polymer composites have focusedmainly on polypropylene and epoxy resin matrix composites [11–16]. And polyester resin could be used for reinforcement due toits advantages like cost effective, easiness in processability, lowerdensity, etc.

Generally, surface modifications enhance the mechanical prop-erties of fibres [19,20]. In the past, there have been few studies onthe surface modification of basalt fibre; however, the good chemi-cal durability of basalt fibre has been mentioned in several articles.

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V. Manikandan et al. / Composites: Part B 43 (2012) 812–818 813

Most researches focus on the applicability, mechanical perfor-mance and interfacial properties of basalt fibre reinforced polymercomposites [9,11–14] but pay little attention to surfacemodifications.

The manufacturing process of the composite is one of the vitalcriteria which decide the strength of the composite. Among allthe fabrication processes the compression moulding method pro-vides better strength to the prepared composite structure [22].Amico et al. [21] found that the compression moulding processof making composite affords better strength in all aspect. In addi-tion, Wanjun et al. [23] also suggested the compression mouldingneither damages nor orients the fibres during processing, whichpreserves the isotropic properties of the composites and reducesthe changes in the physical properties. Hence in this work, com-pression moulding machine was used. Mechanical and chemicalproperties of commercially available basalt fibres Basaltex andKamenny Vek were investigated [24]. It was found that the basaltparticles were worn more slowly than the matrix. There weresome basalt particles with a flat top surface protruding slightlyover the worn surface [25]. The addition of basalt fibre can signif-icantly improve deformation and energy absorption properties ofgeopolymeric concrete, while there is no notable enhancement indynamic compressive strength. Increase of matrix strength resultsin decrease of deformation capacity and increase of energyabsorption capacity for basalt fibre reinforced geopolymeric con-crete [26,27].

Based on a review of the literature, it was found that little infor-mation is available on the use of basalt fibres as a reinforcing agentin polymer matrix. The polyester resin is Hence this work focusedon the studies surface modifications of a basalt fibre that was rein-forced with unsaturated polyester resin.

Table 1Notations used to represent the fibres and the combinations.

Sl.no.

Notationsused

Explanation

1 GUT ‘‘Untreated glass fibre, unsaturated polyestercomposite’’

2 BUT ‘‘Untreated basalt fiber, unsaturated polyestercomposite’’

3 GAT ‘‘Acid treated glass fiber, unsaturated polyestercomposite’’

4 BAT ‘‘Acid treated basalt fiber, unsaturated polyestercomposite’’

5 GBT ‘‘Base treated glass fiber, unsaturated polyestercomposite’’

6 BBT ‘‘Base treated basalt fiber, unsaturated polyestercomposite’’

2. Experimental details

2.1. Materials

Basalt fibre (Plain weave, 220 g/m2) was supplied by ASA.TECH,Austria. E-glass fibre was supplied by G.V.R. Enterprises, Madurai,India. Unsaturated polyester resin, methyl ethyl ketone peroxide(MEKP) and co-napthenate were purchased from Sakthi FibreGlass, Chennai, India. Sodium hydroxide and sulphuric acid werepurchased from the United Scientific Company, Madurai, India.

2.2. Treatment of fibres

The basalt woven fabrics were cut into an approximate size of35 � 35 cm. The fibre was treated by soaking in two solutions,1 N NaOH and 1 N H2SO4, separately for 24 h at room temperature.After this, the fibres were washed several times with distilledwater to remove any NaOH and H2SO4 from the surface of thefibres. Finally, the fibres were dried at room temperature for 24 hbefore the composites were prepared.

2.3. Fabrication of composites

Basalt fibre reinforced polymer matrix composites were fabri-cated using the hand layup method, and unsaturated polyester re-sin was used for the matrix. For a proper chemical reaction, cobaltnaphthenate and methyl ethyl ketone peroxide were used as anaccelerator and a catalyst, respectively. Four layers of basalt fibremats were cut into an approximate size of 35 cm � 35 cm. Thesewere weighed to determine the corresponding 1:1 amount ofunsaturated polyester resin. The polyester resin was cured byincorporating one volume per cent of the methyl ethyl ketone per-oxide (MEKP) catalyst. One volume per cent cobalt naphthenate

(accelerator) was also added. A stirrer was used to homogenisethe mixture. Then, the resin mixture was used to fabricate four lay-ers of basalt fibres with the hand layup technique using a roller.The samples were cured for approximately 24 h at room tempera-ture. A similar procedure was used to prepare the acid-treated ba-salt, the base-treated basalt, the untreated glass, the acid-treatedglass and the base-treated glass fibre reinforced polymer compos-ites. Table 1 shows the glass and basalt fibres and combinations.

2.4. Mechanical property evaluation

2.4.1. Tensile testA tensile test was performed to determine the stress–strain

behaviour of the basalt fibre reinforced polymer composites. Thiswas done using a UTM (3906) with a cross head speed of 2 mm/min according to ASTM D3039. Five samples were taken from eachcombination, and the results were averaged. This showed the ten-sile strength of the polymer composites.

2.4.2. Inter-laminar shear testA short beam test was used to determine the inter-laminar

shear strength (ILSS) of the basalt fibre reinforced polymer com-posites. The ILSS test was conducted on the cured samples usinga Kalpak universal testing machine (080601) with a cross headspeed of 2 mm/min according to ASTM D2344-84.

2.4.3. Impact testAn impact test was used to determine the amount of energy

that was required to break the specimen. An un-notched IzodImpact test was conducted to study the impact energy accordingto ASTM D256. The un-notched specimens were kept in a cantile-ver position, and a pendulum was swung around to break the spec-imen. The impact energy (J) was calculated using a dial gauge thatwas fitted on the machine. Five samples were taken for each test,and the results were averaged.

3. Results and discussion

The fibres can be corroded by diffusion through the matrix,along a degraded interface, or as a result of matrix cracking [17].It is understood that the fibres in the composite materials play amajor role in determining the strength of the material.

The mechanisms of acid and base attacks on basalt and glass fi-bres are different. Acid and base attacks increase in strength withincreasing temperature and time. In accordance with the law ofchemical equilibrium, the concentration influences the rate of thereaction. The chemical composition of basalt and glass determinestheir resistance to water. Chemical resistance does not depend onthe alkali content but instead on the combination of different oxi-

Fig. 2. Effect of fibre combinations on tensile strength.

814 V. Manikandan et al. / Composites: Part B 43 (2012) 812–818

des. Acid resistance is increased by the augmentation of the SiO2

content, and alkali resistance is increased by higher contents ofearth alkali and Al2O3.

The following reactions occur under the action of alkali on thesurfaces of glass and basalt:

�Si� O� R þH2O! �Si� OHþ Rþ þ OH�

�Si� O� Si�þOH� ! �Si� OHþ�Si� O�

The rate of corrosion is not determined by a diffusion-controlledprocess by the active dissolution of the SiO2 network. The loss ofmass is proportional to the time. After a given time, the Si–O skel-eton is destroyed completely. The smooth surface of the fibres be-come rough, and over time, the fibres lose their elasticity andbecome brittle. On the surface of the fibre, a loose layer of reactionproducts are formed. Over time, this layer grows but does not im-pede the entrance of further alkali. The corrosive action of alkalican manifest especially as a large loss of the rigidity of the fibreor the composite.

3.1. Tensile test

A typical stress–strain curve is shown in Fig. 1.The tensile strength value could be taken with the help of in-

built software in the UTM. Fig. 2 shows the tensile strength ofthe glass and basalt fibre reinforced polymer composites. We ob-served that the incorporation of basalt fibres into the unsaturatedpolyester matrix had a considerable effect on its tensile properties.

The acid-treated basalt fibre reinforced composite has a highertensile strength than the other combinations. During the acidtreatment, an ion exchange reaction takes place between the basaltfibre and sulphuric acid until equilibrium is reached. Acid treat-ment of basalt fibres causes an –OH group to form on their sur-faces. Treating basalt fibres with acid can cause two types ofbonding.

1. A covalent bond between the surface of the –OH group and thecarboxylic acid terminated polyester.

2. Hydrogen bonding between the carbonyl group of the ester andthe –OH group of the fibre.

The following chemical reaction occurs during the acid treat-ment of basalt fibres.

Fe2O3 þ 3H2SO4 ! Fe2ðSO4Þ3 þ 3H2O

Fig. 1. Load vs. Ext

Basalt fibre contains 4–4.5% Fe2O3 in its chemical composition.Ferric oxide reacts with sulphuric acid to form ferric sulphates. Theferric sulphates act as a secondary accelerator, which reacts withunsaturated polyester resin to improve the efficiency of the com-posites and the curing reaction and prevents cracking in the curedproduct.

The untreated basalt fibre reinforced composite was 9.88% great-er than the untreated glass fibre reinforced composite (Table 2). Theacid-treated basalt fibre reinforced composite was 24.5% greaterthan the acid-treated glass fibre reinforced composite. Similarly,the base-treated basalt fibre composite was 35.45% greater thebase-treated glass fibre reinforced composite. These results weredue to the alkali attacking the silica network directly; the hydroxylion of the alkali breaks the Si–O–Si linkage. The presence of interme-diate oxides such as MnO2, Fe2O3 and Al2O3 should always improvethe alkali durability of basalt fibres. Therefore, the mechanical prop-erties of the base-treated basalt fibre were greater than those of thebase-treated E-glass fibre.

A scanning electron micrograph of the tensile fractured surfacesof the composites was performed to determine the fracture mech-anism. Figs. 3 and 4 show the fractographs of the acid-treated glassand the basalt fibre reinforced composites, respectively. Fig. 2shows a clear crack formation on the surface of the acid-treatedglass fibre leading to a lack of strength, which was absent in thecase of the acid-treated basalt fibre. The strength of the compositesis governed by the control of flow initiation characteristics. A microcrack is formed, initiated and propagated through the matrix, andwhen it arrives at an interface, it continues along the interface up

ensions graph.

Table 2Comparisons of tensile property of composites.

Comparisons Increased by (%)

GUT > GBT 10.20GAT > GUT 9.539GAT > GBT 20.72BAT > BUT 24.15BAT > BBT 11.01BBT > BUT 11.85

Fig. 3. SEM images of the tensile fracture face of H2SO4-treated glass fibre.

Fig. 4. SEM images of the tensile fracture face of H2SO4-treated basalt fibre.

Fig. 5. Effect of the fibre combinations on shear strength.

Table 3Comparisons of inter-laminar shear strength ofcomposites.



Fig. 6. SEM images of the ILSS fracture face of H2SO4-treated glass fibre.


to fracture of the fibre. After the fibre fractures, the crack propa-gates again into the matrix and then moves to the next interface;this process continues until there is a complete fracture.

Fig. 7. SEM images of the ILSS fracture face of H2SO4-treated basalt fibre.

3.2. Inter-laminar shear test

An inter-laminar shear strength test was performed to assessthe bond strength between the fibre and the matrix resin in thelaminated composites. The characteristics of interface/interphasedepend on both the fibre and the polymer matrix. The optimisationof the mechanical properties of composites is influenced by thebehaviour of this interface/interphase [18]. Fig. 5 shows the in-ter-laminar shear strength of glass and basalt fibre reinforced poly-mer composites.

The interlaminar shear strength of BUT, BAT and BBT was great-er than that of GUT, GAT and GBT, which shows that the adhesionfactor of the combination of the unsaturated polyester resin and

Fig. 9. SEM image of untreated glass fibre.

Fig. 8. Effect of the fibre combinations on impact strength.

Table 4Comparisons of impact strength of composites.



Fig. 10. SEM image of untreated basalt fibre.

Fig. 11. SEM image of NaOH-treated glass fibre.

Fig. 12. SEM image of NaOH-treated basalt fibre.


basalt fibre was greater. The tensile strength, the impact strengthand the SEM images of BFRPC also support this conclusion becausea better interface between the fibre and matrix bonds the fibres to-gether tightly to allow for greater tensile and impact loads. Thebase-treated glass fibre composite had the lowest interlaminarshear strength value of all the combinations because its lower bondstrength may have promoted a large fibre/matrix debonding. Inter-facial debonding can be expected to cause interlaminar crack initi-ation for a composite that has weak fibre/matrix interface bonds.

The untreated basalt fibre reinforced composite was 32.05%greater than the untreated glass fibre reinforced composite (Table3). The acid-treated basalt fibre reinforced composite was 41.47%greater than the acid-treated glass fibre reinforced composite. Sim-ilarly, the base-treated basalt fibre reinforced composite was44.24% greater than the base-treated glass fibre reinforcedcomposite.

Figs. 6 and 7 show the ILSS fracture of glass and basalt fibrereinforced polymer composites. In the acid-treated glass fibre rein-forced composite, there was less bonding between fibre and the re-sin. Fig. 9 shows that the fibre was able to detach easily. Therefore,the strength of this composite was lower than the basalt acid-trea-

ted reinforced composite, in which bonding was strong and the fi-bre did not detach easily.

3.3. Impact test

The impact resistance of a composite is the measure of the totalenergy dissipated in the material before final failure occurs. Fig. 8shows the impact strengths of glass and basalt fibre reinforcedpolymer composites. The acid-treated basalt fibre reinforced lami-nate performed well for impact load. The basalt fibre reinforcedlaminate was also tougher than the GFRP composites. The alkali

Fig. 13. SEM image of H2SO4-treated glass fibre.

Fig. 14. SEM image of H2SO4-treated basalt fibre.


and acid treatments significantly improved the toughness of thebasalt fibre reinforced composites. The acid treatment enhancedthe interlocking ability of the fibre matrix interfaces, which al-lowed for improved energy absorption during impact loading.

We found that the incorporation of basalt fibres into the polyes-ter polymer matrix had a considerable effect on the impact proper-ties (Table 4). We observed that the impact properties of theuntreated basalt fibre reinforced composite were 63.26% greaterthan the untreated glass fibre reinforced composite, and that theimpact properties of the acid-treated basalt fibre reinforced com-posite were 92.51% greater than the acid-treated glass fibre rein-forced composite. Similarly, impact properties of the base-treatedbasalt fibre reinforced composite were 89.20% greater than thebase-treated glass fibre reinforced composite.

4. Scanning electron microscopy

Scanning electron microscopy is an excellent technique forexamining the surface morphology of fibres and the fracture sur-faces of fibre composites. The SEM images in Figs. 9–14 show glassand basalt fibres that were untreated, acid-treated or base-treated.The glass fibre was highly affected by the base treatment (Fig. 11),but both of the untreated fibres showed a smooth surface in themicrograph (Figs. 9 and 10). Therefore, the mechanical behaviourof the base-treated glass fibre was lower than other combinations,but the base-treated basalt fibre’s surface was not affected by thetreatment (Fig. 12). The base-treated basalt fibre reinforced com-posites showed greater mechanical strength than the base-treatedglass fibre reinforced polymer composites. The surface of the glass

fibre was affected by acid treatment (Fig. 13), but the acid did notpenetrate the interior. Therefore, the mechanical strength of theacid-treated glass was greater, but it was less in the acid-treatedbasalt fibre.

5. Conclusion

We conclude that:

1. The performance of basalt fibre reinforced composites withunsaturated polyester was superior to the glass fibre reinforcedcomposites.

2. The tensile tests showed that acid-treated basalt fibre rein-forced composite had higher tensile strength values than othercombinations.

3. The glass fibre composite was much more affected by the basetreatment than the basalt fibre reinforced composites.

4. The impact tests showed that the acid-treated basalt fibre rein-forced composite had greater impact strength.

5. Overall, the study showed that the reinforcement of basalt fibrecomposites created a new material with properties that aregenerally superior to glass fibre reinforced polymer composites,depending on the loading conditions.

Acknowledgements

We gratefully acknowledge the financial assistance provided byDST (SERC): SR/S3/ME/0038/2007, GOVERNMENT OF INDIA for thiswork. We also thank the Centre for Composite Material, Depart-ment of Mechanical Engineering, Kalasalingam University, andKrishnankoil for their help in completing this work.

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