Composite Structures 94 (2012) 11651174

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Composite Structures
journal homepage: www.elsevier.com/locate/compstruct

Static and fatigue characterisation of new basalt bre reinforced composites

C. Colombo a,, L. Vergani a, M. Burman b
a b

Department of Mechanical Engineering, Politecnico di Milano, Via La Masa 1, 20156 Milano, Italy Aeronautical and Vehicles Engineering Department, Royal Institute of Technology (KTH), SE-100 44 Stockholm, Sweden

a r t i c l e

i n f o

a b s t r a c t
Basalt reinforced composites are recently developed materials. These mineral amorphous bres are a valid alternative to carbon bres for their lower cost, and to glass bres for their strength. In order to use basalt reinforced composites for structural applications, it is necessary to perform a mechanical characterisation. With this aim in the present work experimental results of several static and fatigue tests are described. Two polymeric matrices are taken into account, vinylester and epoxy, to assess their inuence on the evaluated parameters. In parallel to these mechanical tests, also the thermal answer of the specimens to mechanical loads is evaluated by means of thermography. This experimental technique allows dening the composite local heating during the application of mechanical loads and its behaviour in details. Final discussion on obtained results is proposed focussing the attention on basalt bre composite behaviour, and comparing mechanical properties of BFRP with other composite materials in glass and carbon bres. 2011 Elsevier Ltd. All rights reserved.

Article history: Available online 14 October 2011 Keywords: Basalt bre reinforcement Fatigue Thermographic analysis

1. Introduction In present times, the use of composite structures is becoming more and more important and their employ can be planned for lightweight and performing structures. Different types of composite materials have recently been introduced and studied, in different scales from macro to nano composites. Considering long bre reinforced composites, together with the more diffused glass and carbon bre, other kinds of reinforces have been introduced and discussed in the literature, such as aramid, ceramic, and polyamide, but also natural bres as ax, hemp or sisal [1]. The attention of the present work is focused on basalt reinforce bres. Basalt is a mineral of volcanic origin, dark or black; its rocks are heavy, tough and resistant and they can present a porphyry, microcrystalline or glassy structure. Basalt is the most abundant rock type in Earths crust; also, most of the ocean oors are predominantly made up of basalt. Basalts composition, however, is slightly variable and not always suitable for the manufacture of bres, due to the presence or absence of trace elements [1]. The rst trials to produce basalt bres (BF) go back to 1923 in US (Paul Dh patent, as cited in [2]); after World War II researches were developed in US, Europe and Soviet Union to get the bres extruded and study the rst applications in military and aerospace elds. From 1995, the technology for bres production was declassied and civilian research begun. The production of bres has therefore only recently been developed, in the last decades, melting basalt at
Corresponding author. Tel.: +39 02 23998667.
E-mail address: chiara.colombo@mecc.polimi.it (C. Colombo). 0263-8223/$ - see front matter 2011 Elsevier Ltd. All rights reserved. doi:10.1016/j.compstruct.2011.10.007

a temperature around 1400 C and then extruding it into bushing, in ne bres shape of 913 lm diameter [3]. Applications of BF are now widely spread in different elds, not only mechanical, for their wide range of good properties. Thanks to their thermal properties, BF offer an excellent economic alternative to other high-temperature-resistant bres (carbon) and are typically utilised in heat shields, thermal insulting barriers and as re protection [4]. In the building eld, BF are also used for the production of cements, in which basalt in mixed in the matrix as short bre (staple) or cut (chopped) to improve structural strength and lower the weight [5]. Basalt is also used to replace asbestos in almost all its possible applications: as insulating material (since basalt has three times asbestos heat insulating properties) or as friction material. In automotive industry, the facing reinforcements used in brakes and clutches until recent years were made of asbestos because of its thermal resistance, strength, high friction coefcient and low wear rate. However, crystalline nature of asbestos causes very ne particles to be formed when its bres are fractured [6]. The breathability of these ne asbestos bres led to the removal of asbestos from friction materials (limit diameter for breathability %3 lm [7]). Because of its good electrical insulating properties, basalt bres are also used, for instance, for printed circuit boards and extra ne resistant insulation for electrical cables and underground ducts [8]. Last but not the least, also in shipbuilding eld basalt bres nd an application. Thanks to their high seawater and UV radiation resistance, basalt composites are also used as sail reinforcement. In the present work, basalt bres reinforced composites used in experimental analyses are manufactured for a naval application, the

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manufacture of ship hulls. Indeed, together with their favourable strengthweight ratio, as most of the composites, basalt reinforced composites experience moreover a good resistance to impact. A comparison of basalt bre properties with E/S-glass and carbon bres, deeply used in composites production, is useful for understanding basalt bre reinforced plastics (BFRP) potential applications. In Table 1a, mechanical properties of basalt bres are reported [9]: these reinforcement bres are suitable to ll the gap between glass bres and the more resistant but much more expensive carbon bres. Indeed, basalt bres show better mechanical properties than breglass, especially with respect to E-glass; their mechanical properties are more comparable with S-glass type. Moreover, they are signicantly cheaper than carbon bres. Comparing basalt to glass bres, these last show a superiority in terms of cost-performance ratio. In Table 1b thermal properties of BF are compared with glass bres: basalt can be used over a wider range of temperatures with respect to glass bres [10]. Other properties of basalt bres are related to its chemical structure: if compared glass bres, BF are more resistant to acid and suffer less degradation by water and alkalis [8]. No chemical additives or solvents are required in the production process. Therefore, unlike some breglass applications, basalt bre products do not release chemical elements when heated, since they are completely natural. For the same reason, the production process itself is environmentally friendly; moreover, basalt can be recycled. Aim of the present work is to experimentally study the mechanical properties of BF reinforced composites. Extremely few and very recent works are present in the literature dealing with BF, especially dealing with their fatigue behaviour. One of these few works is [11], presenting a comparison in terms of mechanical properties between composites with this kind of bres and other reinforcement bres (glass, carbon and hybrid cases among these). Two matrices are here taken into account, vinylester and epoxy, to assess their inuence on the evaluated parameters. Different kinds of mechanical tests are planned and performed: static tensile and compression tests, static delamination tests, classical and stepwise fatigue tests. In this way, the static and fatigue mechanical behaviour of the composite can be completely studied and understood. In parallel to these mechanical tests, also the thermal answer of the specimens to mechanical loads is evaluated by means of thermography. This experimental full-eld non contacting technique allows dening the composite local heating during the application of mechanical loads and its behaviour in details, as already dened in the literature [12], where thermography is generally applied to the study of fatigue life of homogeneous
Table 1 Basalt bre properties: comparisons with carbon and glass. Glass bres Basalt a. Mechanical properties Tensile strength (MPa) Elastic modulus (MPa) Elongation at break (%) Density (g/cm3) Price (year 2007) (USD/kg) 4840 89,000 3.1 2.8 2.5 E-glass 3450 72,400 4.7 2.6 1.1

materials [13]. Thermography is applied, in the present work, as an experimental technique to assess fatigue behaviour and damage in composites. Final discussion on obtained results is proposed focussing the attention on basalt bre composite behaviour, and comparing mechanical properties of BFRP with other composite materials in glass and carbon bres. 2. Sample manufacturing Two types of panels are manufactured, using the same reinforcement bres. BF are provided by Basaltex as biaxial fabrics (type BAS BI 600) [14]. Lamination sequence is:

0 =90 = 45 = 45 2s

This symmetrical lamination sequence was selected to avoid, or at least reduce, problems of strains coupling, which can arise not only from the application of external loads but also during the stage of laminate consolidation, and in both cases they are responsible for body distortions. Two kinds of matrices are used for the manufacturing: 1. a vinylester resin (DION VINYLESTER UN 1866) and its additives; 2. an epoxy resin (RenLam LY 113 100) with its hardener (Ren HY). For these different resins used in matrices manufacturing, panels and specimens are identied with two acronyms: BV (Basalt bre reinforced composite with Vinylester matrix) and BE (Basalt bre reinforced composites with Epoxy matrix). For both the two kinds of panels, bre volume ratio (Vf) is 50%. The technique used for panels manufacturing is the vacuum infusion process. Panels dimension is 30 30 cm2 in order to reduce the amount of resin and succeed in a short time to thoroughly mix the components together. Panels thickness is nominally 3.5 mm; once they are ready, rectangular specimens are cut by a saw. 3. Description of experimental tests The experimental tests carried out on the basalt reinforced composites samples are: static tensile tests; static compression tests; static delamination tests; fatigue tests; stepwise tests.

During static tensile and dynamic tests, the composite behaviour was monitored also from the thermal standpoint by means

Carbon bres S-glass 4580 85,500 5.6 2.5 1.5 Basalt High strength 3500 240,000 1.25 1.75 30 High modulus 25004000 350,000650,000 0.5 1.95 Glass bres 650 480 60 0.0340.04 5.4

b. Thermal properties Maximum application temperature (C) Sustained operating temperature (C) Minimum operating temperature (C) Thermal conductivity (W/m K) Thermal expansion coefcient (ppm/C)

982 820 260 0.0310.038 8

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of a thermocamera. Details of the experimental tests are described in the following paragraphs. 3.1. Static tests Static tensile tests are performed following ASTM D3039/ D3039M standard [15]. Two testing machines are used, since tests are performed in part at KTH and in part at Politecnico: Instron 4505 with a load cell of 100 kN, equipped with an extensometer (type Instron 2620-601, base length = 50 mm); MTS Alliance RF150 with a load cell of 100 kN, for tests monitored by a thermocamera. All static tensile tests are carried out at room temperature, under standard humidity conditions. Tests are performed in displacement control, at 2 mm/min speed of the crosshead. Specimen dimensions are 25 250 mm2; all the specimens are provided with tabs (length = 50 mm) to prevent premature failure of the sample at the grips. Static compression tests are performed following ASTM D3410/ D3410M standard [16]. Testing machine Instron 4505 is used with a special compression xture. This additional equipment, prescribed by the standard, consists in rectangular tapered wedge grips and allows specimen alignment with respect to the longitudinal axis in the test xture. An excessive bending, indeed, can cause premature failure and highly inaccurate determination of the elasticity modulus. Regarding static delamination tests, ASTM D5528-01 standard is followed [17]: this standard refers to mode I opening and indicates the calculation of the interlaminate fracture toughness, GIC, for bre-reinforced composites. Used specimens are double cantilever beams (DCB): to prepare such rectangular specimens, a non-adhesive insert in the midplane of the lamina was included during plate manufacturing. This ensures a controlled delamination onset. The standard requires that the specimen is a laminate with an even number of plies and that the delamination growth occurs in 0 direction, that is non adhesive insert must be placed between two 0 unidirectional plies. This implies that the resistance to delamination is provided by the development of bre bridging, and this effect is not shown between plies of dissimilar orientation. For this reason, and only for delamination tests, the stacking sequence of these specimens for delamination tests is changed into [[0/90/+45/ 45]s]s; insert length is 63 mm. DCB specimen is then loaded in opening mode by a couple of hinge tabs attached to the end of the specimen. Two plastic strips, one at each specimen side, are connected to the hinges, xed by small bolts. At the other sides, strips are placed into the grips of the loading machine, ensuring that the specimen is aligned and centred. At the beginning of the test, the specimen is already open thanks to the non adhesive insert, so the applied forces are not very high: the strips compliance is much bigger than that of the opened specimen. Opening forces are applied by a tensile testing machine, in displacement control, at 4 mm/min. During the test, applied load and delamination length are monitored and recorded. Specimens are also prepared by colouring their lateral side with a white paint and then accurately drawing marks each 5 mm. Load is applied in steps during testing: each time crack tip reaches a mark, the load is manually stopped and crack length is measured. Test is stopped when delamination reaches 45 mm of propagation from the precrack tip. The used testing machine is an Instron 5567 with a 10 kN load cell. An optical microscope, placed in front of the specimen into the tensile test, is used to observe the propagation of the delamination front on the specimen edge. Specimen dimensions are

25 125 mm2; all the specimens are provided with tabs (length = 50 mm). Experimental test setup is shown in Fig. 1. The evaluation of GIC is performed by following the beam theory (BT) and the modied beam theory (MBT), respectively indicated in the ASTM standard [17] for a perfectly or not completely built in cantilever beam. 3.2. Fatigue and stepwise tests To perform fatigue and stepwise tests, ASTM D3479 standard is followed [18] and the following hydraulic testing machines are used: MTS 810 with a 100 kN load cell for BV specimens; Instron 5811 with a 20 kN load cell type for BE composites. Aim of the fatigue tests is to describe the fatigue behaviour and to provide for the rmaxlog(Nf) curve of the considered basalt bre reinforced composite materials. Fatigue parameters for testing basalt composite specimens are: constant stress amplitude; stress ratio R = rmin/rmax = 0.1; frequency: f = 10 Hz; number of cycles to consider run out the specimen: Nro = 5 106 cycles.

Specimens are similar to the ones used for static tensile tests (25 250 mm, with tabs of 50 mm). In parallel to fatigue classical tests, also a stepwise test is performed on an un-cycled specimen. Stepwise tests consist in fatigue tests with different blocks of cycles at variable stress amplitude, at 20 Hz. During these tests, a thermocamera is used to monitor surface temperature. 4. Thermography: static and fatigue application Damage in composites is rather complex compared to isotropic and homogeneous materials, due to the different kinds of damage (bre failure, matrix cracking, interfacial debonding, transverseply cracking and delamination). In the present work thermography is used as experimental technique to quantitatively evaluate composite damage by measuring the surface temperature. This technique allows detecting a full eld real time measurement of the surface temperature in a component or specimen subjected to a static or dynamic load. In the literature it is possible to nd some studies about the application of thermoelasticity to com-

Fig. 1. Experimental setup for delamination tests.

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posite specimens, most of all about glass bre composites [12], but the application of this experimental technique is completely new for basalt bre reinforced composites. In this paragraph, after the equipment and the methodology used in the experimental tests (in the literature applied to homogeneous materials) are described. 4.1. Equipment The basic equipment for thermography is the infrared thermal camera (type FLIR Titanium SC7000 [19]). The main technical features of this type are: sensors (InSb), type Focal Plane Array, 320 256 pixel; waveband: 2.55 lm; full frame rate: up to 380 Hz; thermal sensitivity: 25 m K.

ture variation is negative. The specimen shows a globally elastic behaviour; this phase is regulated by the theory of thermoelasticity [21]. Part II: micro-damages occur in the specimen starting from the existing micro-defects, even if at macroscopic point of view the material does not show any damage. In this phase, the linear proportionality between the applied stresses and temperature is missing. The temperature trend decreases not linearly, till a minimum value. This point corresponds to a balance between the energy spent for elastic deformation (cooling the specimen) and the energy absorbed by the composite to increase defects and damages (heating the specimen). Part III: the material damage is spreading out and damage propagation inside the specimen leads it to failure; when propagation nally becomes instable, a sudden heat release occurs. In [22], the authors assessed the rst deviation from linearity before that it is visible in the classical tensile test, on plastic specimens; they associated the corresponding stress value to the fatigue limit. For composite materials, it is not possible to dene a fatigue limit, because the degradation of these materials is always not reversible [23]. However, the end of the thermoelastic phase could be related, also for composites, to a stress value (rD in Fig. 2), which can identify the initiation of a different kind of damage. 4.3. Thermography for cyclic tests of homogeneous materials Experimental observations [13] of the surface temperature in homogeneous material specimens indicated, for fatigue tests, a trend of temperature variation (dened as the difference between the instantaneous temperature and the initial temperature, averaged on the specimen surface during the fatigue test). In particular, the mean temperature in a loading cycle, DTmean, increases during the initial phase (around 10% of the entire lifespan), then remains almost constant (stabilised), until short time before the failure. It nally shows a further increase immediately before failure. Moreover, [13] showed that during fatigue tests, for a given test frequency and stress ratio, DTmean value referred to the number of cycles is a function of the applied stress. Indeed, the higher is the applied load, the higher is the stabilisation temperature and the rate of temperature increase with the number of cycles. Based on these experimental observations, [13] proposed a methodology to evaluate fatigue behaviour of a homogeneous material, by applying stepwise fatigue loads and monitoring the thermal variation of the specimen surface. The procedure consists in loading a specimen by blocks of cycles at different increasing amplitudes till specimen failure. Each block of cycles, at constant stress amplitude, is run for a sufcient number of cycles to reach a stabilisation temperature. The different DTmean/DN ratios are collected at each stress level. All these values lay on a straight line in the (DTmean/DN) rmax graph: by adding a tting linear trend, it is therefore possible to nd the intercept with rmax axis. This value, according to [13], corresponds to the fatigue limit of homogeneous materials. The D-mode technique is another method used to determine the fatigue limit of homogeneous materials [24]. This technique consists in analysing the dissipated energy due to phenomena of fatigue damaging by stepwise tests. Cracks propagation and local plastic behaviour evidence a change in the dissipated energy (D), which presents a double linear trend. Indeed, D is linearly proportional to the applied load till the material is in the elastic behaviour, or at least fatigue phenomena of damaging are negligible with respect to the total dissipated energy. When, on the contrary, more important fatigue phenomena occur, the increase of D with respect to the applied load is still linear but with a second and

Infrared thermal cameras are used to detect radiation (heat) emitted by a body in the infrared spectrum. The thermal camera records a matrix (image) of surface temperatures in the analysed area. During tests, the thermal camera is placed in front of the specimens, at a distance of about 250 mm that can vary based on the specimen region to be detected. The IR camera is connected to a laptop, where acquired data are stored. ALTAIR, the software provided with the thermal camera, is used both for thermocamera conguration and control, and for the elaboration of thermal images during data post-processing. During data acquisition, the thermal camera is linked to the load cell of the testing machine by means of the so-called lock-in module. This allows a simultaneous acquisition of thermal and mechanical data, and also provides for a lter against noise signals. 4.2. Thermography for static tests of homogeneous materials Studies are present in the literature to relate static tensile behaviour (mechanical and thermal) to fatigue properties of homogeneous materials, for instance steel and aluminium alloys. Surface temperature of a material under monotonic and static tensile load has a complex trend during time, which can be divided in three parts (Fig. 2) [20]: Part I: the temperature variation (DT = T T0, the difference between the instantaneous and the initial temperature) during time can be schematised by a perfectly decreasing straight line; in parallel, the load-time trend is also linear elastic. In this phase, the specimen change in volume, directly proportional to the change in strain, is positive, while the tempera-

Part I Part II

Part III

tD

Time

Fig. 2. Schematisation of applied stress r and temperature variation DT in function of time, during a static tensile test.

T=T-Tt=0

Stress

C. Colombo et al. / Composite Structures 94 (2012) 11651174 Table 2 Results from experimental static tensile and compression tests. BV Ultimate tensile strength, rUT (MPa) Elastic modulus, E (MPa) Ultimate compression strength, |rUC| (MPa) Strain at failure, compression |efC| (mm/mm) 317.3 8.5 17,902 782 169.3 14.1 1.41 0.11 BE 409.2 9.2 20,338 738 311.8 16.7 2.62 0.14

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Percentage increase (%) +29.0 +13.6 +84.3 +86.0

Displacement [mm]

(a) 450
400 350

BV BE

(b)
Stress [MPa]

0 0 -50 2 4 6 8

Stress [MPa]

-100 -150 -200 -250 -300

300 250 200 150 100 50 0 0 0.005 0.01 0.015 0.02 0.025 0.03

-350

BV BE

Strain [mm/mm]
Fig. 3. Comparison between typically obtained static curves for BV and BE specimens: (a) tensile and (b) compression curves.

Fig. 4. Broken specimens after static tensile tests: (a) BV and (b) BE specimens.

higher slope. The software, provided with the thermal camera, can perform a post-processing of the experimental thermal data collected during stepwise tests. In the present paper, these techniques (static, stepwise with DTmean/DN and with the D-mode) are applied in order to evaluate the stress corresponding to the damage initiation (rD). 5. Results In this paragraph, results of the experimental tests are presented, rstly from the only mechanical standpoint, and then from the thermographic point of view. 5.1. Tensile and compression characterisation of the composites Table 2 shows the results from static tensile and compression tests. This table shows that the use of epoxy instead of vinylester for basalt composite matrix increases mechanical static (tensile and compression) properties. Considering, for instance, the ultimate tensile strength, BE specimens showed an increase of

29% with respect to BV composites. In the same way, all the other characteristics show improvements, especially in the compression behaviour, where this increase is more evident (+85%). Indeed, in this case, the matrix rather than the bres provides the resistance. Plots in Fig. 3 show a comparison between the static tensile and compression curves of the two tested specimens. From Fig. 3a, it is evident that the BV and BE specimens show a similar slope in the linear region (the increase in E is only 13%), while increasing the applied load, the curves diverge and present different trends. If the BV specimen fails with a at trend in the re plot, the BE presents a sudden failure, although at higher load. Broken specimens during tensile tests are shown in Fig. 4; in the images, white marks on specimens indicate the central region where extensometer was placed during testing. In both kind of composites, failure during tensile tests occurs since delamination started from the underlying layers, inclined of 45 angle. This causes a swelling in the sample along the thickness. However, referring to BV composite, specimens are more open along the thickness and bres tend to separate from the matrix, as shown in Fig. 4a. BE specimens, instead, are more compact and show

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C. Colombo et al. / Composite Structures 94 (2012) 11651174 Table 3 Summary of the fatigue tests on BV and BE specimens. Specimen BV1 BV2 BV3 BV4 BV5 BV6 BV7 BV8 BV9 BV10

rmax (MPa)
175 150 125 125 110 110 90 80 75 75

Nf (cycles) 1189 5778 23,671 21,659 82,547 171,314 321,543 1585,199 Run out Run out

Specimen BE1 BE2 BE3 BE4 BE5 BE6 BE7 BE8 BE9 BE10

rmax (MPa)
250 210 180 180 180 165 150 150 120 84

Nf (cycles) 1032 12,191 5477 4698 11,850 40,957 98,836 62,022 4468,365 Run out

Fig. 5. Broken BV and BE specimens after static compression tests.

Table 4 Results of the tensile static tests on BV run-out specimens. Specimen BV9 BV10 Average % Difference with non-cycled specimens

some oblique lines along which the failure occurs (Fig. 4b). In conclusion, tensile tests indicated that epoxy resin has a better adhesion with basalt bres if compared to vinylester resin. Considering Fig. 3b and the direct comparison between BV and BE behaviour under compression loads, r-displacement plots show a similar trend for the two composites: only, the BE curve is superior. Failure mode in compression for these specimens is the same for both composites (Fig. 5). In fact, as already mentioned, in compression tests what mainly determines the material response are the matrix properties. Specimens failed in TAT mode (failure mode: transverse shear, failure area: at grip/tab, failure location: top), as dened in ASTM D3410/D3410M standard. From the presented results of static tests, it is evident that the BE specimens show higher mechanical properties. For this reason, higher attention is focussed in this work on such kind of composite: delamination tests were therefore performed only on BE specimens. 5.2. Delamination characterisation of the composites An example of interlaminar (delamination) result is described in Fig. 6. In these plots the application of modied beam theory (MBT) is shown, in order to obtain more precise results with respect to the simple beam theory (BT), since the specimen is not xed in the out of plane direction. In Fig. 6a, an example of a C1/3a (compliancecrack length) plot is shown to evaluate |D| value. This value is used to correct GIC, calculated according to BT, and to re-evaluate it by MBT. In Fig. 6b, indeed, these two values of GIC are shown for the same specimen: the difference in GIC evaluations shows a high inuence of the

rUT (MPa)
208.3 205.0 207.6 34.9

E (MPa) 18,037 16,921 17,479 2.4

out-of-plane displacements. The interlaminar test was repeated on a second specimen: the average value of these two experimental results was GIC = 644 N/m. 5.3. Fatigue tests Traditional fatigue tests (rmaxlog Nf curves) are performed on BV and BE composite specimens: in Table 3 and Fig. 7 a summary of the fatigue results is reported. From these plots, data show a very low scattering and the straight line tting experimental data presents a good regression parameter. In the plots, also static data, rUT, are included (i.e. for Nf = 1): the tting curve is forced to pass from this point in the rmaxlog Nf plot. Run-out specimens from the BV series were also tested to evaluate residual strength and stiffness. Results in terms of rut and E are shown in Table 4: if the average of these parameters is considered, some comparisons can be proposed with the non-cycled specimens. Static strength is decreased of 35%, while stiffness (Youngs modulus) is kept almost constant (2.4%). The deep decrease in strength is symptomatic of the fatigue damage cumulated by the specimen during cycling.

(a) 0.16
0.14 0.12 y = 1.2176x + 0.022 R = 0.9541
2

(b) 1200
1000 800

C1/3 [m/N]

G [N/m]

0.1 0.08 0.06 0.04 0.02 0

600 400 200 0 0.04

MBT BT GIC (MBT) GIC (BT) 0.06 0.08 0.1

-0.025

0.025

0.05

0.075

0.1

0.125

Crack length, a [m]

Crack length, a [m]

Fig. 6. Example of application of the modied beam theory /MBT) to GIC calculation on a BE specimen: (a) Ca and (b) Ga plot.

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(a)
max [MPa]

350 300 250 200 150 100 50 0 1.E+00 1.E+02 1.E+04 1.E+06
Static Fatigue Run out Linear regression

(b) 450
400 350

Static tests Exp results Run out Linear regression

max [MPa]

300 250 200 150 100 50 0 1.E+00 1.E+02 1.E+04 1.E+06

Nf [cycles]
Fig. 7. rmaxlog Nf diagrams: (a) BV and (b) BE specimens.

Nf [cycles]

Before proposing discussions and comparisons on fatigue results, thermographic results are now exposed. 5.4. Thermographic data analysis In this paragraph, results related to the application of thermography are presented. Two kinds of tests are performed, static and stepwise, thermodynamically monitored as described in Section 4. These tests were performed only on BE specimens, since the ones with epoxy matrix evidenced higher static and fatigue mechanical properties. Due to the low data scatter, that this composite showed in the static and fatigue tests, two specimens were thermographically monitored, and one underwent stepwise fatigue cycling. Considering static tests, results of the thermographic tests are plotted in the double scaled plot of Fig. 8 for one of the non-cycled (virgin) BE specimen: in this plot, applied static stress r and variation of temperature with respect to the initial value (DT) are plotted in function of time t. It should be mentioned that the used software for thermographic data analysis (ALTAIR) allows selecting a region of the specimen and to plot the trend of the average surface temperature in function of the acquired frames (time). Moreover, the chosen area on the specimens does not affect temperature trend. Considering, for instance, two or more different regions of the specimens, chosen simply avoiding borders, the trends are similar: in particular, the end of the linear part happens at the same instant, as well as the minimum temperature variation. In this light, for the following data processing and thermographic results, only one area covering the entire central part of the specimen was taken into consideration. Going back to Fig. 8, a linear regression of the rst part of the curve, trying to include as many thermal data as possible, as well as keeping increasing the value of R2 regression parameter. As R2 decreased, no more data were taken into consideration. In this same graph, the thermo-mechanical behaviour of a BE specimen is shown: a minimum decrease of almost 0.4 C occurs before a further and nal increase. The rst part of the DTt curve is the most interesting one according to [13]. In the rst stage of loading, indeed, after a non linear initial part of the curve probably due to the stabilisation at the grips of the testing machine, it is possible to identify a linear trend and a constant slope of temperature decreasing. It also corresponds to the linear part of the curve rt. It is possible to identify the end of this linear part at the instant of time, in correspondence of which rD can be evaluated on the rt curve. After this linear part in DTt curve, the slope of the curve is changing till a minimum, evidencing an almost at trend. During this second phase (part II in Fig. 2), internal modications in the

450 400 350 300

Stress Temperature Interpolated data (T) Linear regression

0 -0.05 -0.1

y = -0.0026x - 0.0238 R = 0.9896

2

-0.15 -0.2 -0.25 -0.3 -0.35 -0.4 -0.45

[MPa]

250 200 150 100

D = 68.5 MPa50

0 0 50 100 150 200 250 300

t [s]
Fig. 8. Stress and temperature variation plots in function of time, for static tests for a BE specimen.

composite structure happen, which make the global behaviour of the specimen to be no more linear in the temperature domain; such a behaviour is not detectable in the rt curve. After the minimum, the increase in temperature (gradient in the DTt graph) is higher till the nal failure. rD evaluation can therefore be performed, as indicated in Fig. 8, and a value of 68.5 MPa is obtained. A very similar trend was obtained for the second tested BE specimen, thermographically monitored, and a second value of 69.5 MPa obtained. This indicates that the behaviour of this material is very repeatable, not only from the mechanical, but also from the thermal point of view. During the stepwise test, the surface temperature of the specimen was recorded by the thermocamera. Acquired matrices of temperature in function of the time are analysed in the post-processing phase to:

Table 5 Scheme of loading and evaluated temperatures for stepwise testing.

rmax (MPa)
40 50 60 70 90 110 130

N (cycles) 3000 10,000 10,000 10,000 10,000 10,000 4227

T [C]

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45 40 35

0.2

0.15

T mean [C]

25 20 15 10 5 0 0 20000 40000 60000

T [C]

30

0.1

0.05

0 0 5 10 15

N [cycles]
Fig. 9. Stepwise temperature trend.

N [cycles]

0.3

0.004

Exp data Linear fitting

0.25 0.003 0.2 0.0035

Tmean /N [C/cycle]

T amplitude [C]

y = 7E-05x - 0.0039 2 R = 0.9998

0.0025 0.002 0.0015 0.001 0.0005

0.15

y = 0.0025x - 0.0279 2 R = 0.9542

0.1

y = 1E-05x - 0.0002 R2 = 0.9435

0.05

0 0 50 100 150

D=68.5MPa
0 40 50 60 70 80 90 100 110

max [MPa]
Fig. 10. Variation of amplitude temperature, function of maximum applied stress.

max [MPa]
Fig. 11. DTmean/DN in function of rmax for a BE specimen: double linear interpolation and identication of rD.

check the trend of the specimen answer in terms of average temperature variation during time in function of the applied stress (DTmean/DN rmax); evaluate heat dissipation of the specimen, out of phase with respect to the load cell signal, by means of the D-mode technique. The specimen is subjected to block of cycles, following the history of load indicated in Table 5. The rst loading step has a lower number of cycles (3000): these initial cycles are necessary to initialise the specimen temperature and to avoid inuence of the external environment. The following steps have longer durations, to globally check the DTmean trend. Test is stopped when the specimen failed. In Fig. 9 the global trend of the mean temperature variation with respect to the initial is shown, as well as each thermal cycle underwent by the specimen (four data are available for each cycle). Before presenting the results in terms of DTmean, it is worthy to mention that a check on temperature amplitude during each block of cycles was also performed, as shown in Fig. 10. This plot of DTamplitudermax clearly shows that the trend of DTamplitude is linear with load application, and that only the mean trend of the temperature can be used to evaluate the fatigue behaviour. No

4 3.5 3 2.5 2

D mode

D=85.8MPa
1.5 1 0.5 0 40 60 80 100 120 140
y = 0.0005x + 0.0133 R2 = 0.75 y = 0.041x - 3.46

Stress [MPa]
Fig. 12. D-mode in function of rmax a BE specimen: double linear interpolation and identication of rD.

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information about fatigue behaviour can therefore be evinced from the amplitude trend. Considering DTmean, two possible methods are applied to determine rD for BE composite. The rst considered method required the detection of the ratio DTmean/DN in function of rmax, as in Fig. 11. In this plot, the trend of experimental data can easily be tted by a double linear interpolation: the intercept between these two straight lines identies a stress value for damage initiation (rD = 68.5 MPa). This evaluated value is in complete agreement with the one from the static thermally monitored test. The second method taken into account to understand the behaviour of BE composite under stepwise cycling, considering the same mentioned specimen, is the D-mode technique. Also in this case, a double linear trend can be evidenced in the evaluated dissipated energy, as shown in Fig. 12. It shows the trend of Dmode in function of rmax: it is possible to clearly evidence two linear regions. According to literature [24], the stress corresponding to the intercept of the two lines (rD = 85.8 MPa), i.e. the separation between the two composite behaviour phases, can also be related to the fatigue strength. From the thermal data, it is therefore evident that for a value of stress 70 MPa < rD < 85 MPa the damage mode changes both from a qualitative and quantitative point of view. If a normalisation with respect to the ultimate tensile strength rUT is considered, the range of rD/rUT is therefore between 0.17 and 0.21. 6. Discussion Different experimental results have been reported in the previous paragraph, dealing with the proposed mechanical tests on BF reinforced composites, and many points of discussion raised. The plot in Fig. 13 shows all the obtained results as normalised values rmax/rUT. First of all, it is evident a similar trend of fatigue curves of BV and BE specimens. A common tting straight line (the dashed line) is plotted, considering all the available experimental fatigue data; this line is forced to pass from the static strength (rmax/rUT = 1). The tting line has the following equation:

decay of the mechanical properties of BFR composite with fatigue loads, thus synonym of a continuous mechanical and irreversible damage in the material, as typical for most of the composites. Always considering Fig. 13, a further consideration seems interesting to be proposed. At higher number of cycles and low stress levels, specimens fail deviating from the linear trend, as it is also underlined by the presence of run-out specimens already at 0.24 rmax/rUT, which can only partially justied by the scatter. It seems that, decreasing stress level, a further linear trend could be used in specimens interpolation. For this reason, therefore, a second possible interpolation of the fatigue trend is shown (the bi-linear trend in Fig. 13). For high cycle fatigue (Nf > 106), it seems indeed that the damage of the specimen can change with respect to the rst part of the fatigue curve, being always linear, but changing slope. Hypotheses on the physical meaning of this behaviour can be related to the predominance of different modes of mechanical properties degradation. This decay, at higher stress levels can be related to the creation of macro cracks or brematrix debonding, while at lower stress levels to micro cracks, for instance generated from pre-existing defects. Further experimental tests at high number of cycles are required to deepen this theory. Considering the results of the thermal observations, it is possible to summarise the estimations of rD: 69.0 MPa from the static thermoelastic observations; 68.5 MPa from the DTmean/DN rmax plot; 85.8 MPa from the D-mode technique. The rst two estimations completely agree each other, while the third one overestimates the evaluation of rD of around 20%. It is therefore now important to discuss the meaning of this rD in the light of the obtained fatigue results of Fig. 13. This stress value seems correspond to the intercept of the two lines used in the bi-linear data interpolation: it can be related to the transition point between different kinds of composite damage mechanisms. Considering approximately a number of cycles of 3 106, the corresponding stress is 71 MPa (rmax/rUT = 0.17), similar to the estimated rD value from the used thermographic methods. In order to fully compare the obtained results with other reinforced composites widely spread nowadays, in Fig. 13 two curves related to glass (GF) and carbon (CF) bre reinforcement are also indicated. The curve related to GF has a slope of 0.1 in the rmax/rUT log(Nf) plot and it is taken from a previous work [25], obtained by different experimental data for glass bre composites with multiple stacking sequences. In that work, indeed, it was evidenced a global trend for GF reinforced composites in fatigue life and a constant decay of their mechanical properties during cycling. Considering CF, this decay is less evident: the line plotted in Fig. 13 representing CFRP is higher with respect to the two previously mentioned kinds of composites, thus indicating a very small damaging in fatigue. Slope of these kinds of composites, 0.05, is obtained considering the experimental works by [26]. As it is possible to see, BFRP show a net lower trend with respect to CF (60% in the slope). It is also slightly lower with respect to GF (20% in the slope). However, the use of basalt bre as reinforcement in composites production can be supported by their favourable ratio between performances and costs. 7. Conclusions In this work, a recently developed composite is taken into account, with basalt bre reinforcement. Very few data are available in the literature dealing with this composite, so, a static and fatigue characterisation of the mechanical and thermal properties was performed. Two kinds of matrices are taken into account, vinylester and epoxy. Tensile and compression static tests, delamination

rmax 1 0:1275 logN f rUT

Moreover, all the experimental fatigue data, both for BV and BE, have a very low scatter with respect to the average trend, as indicated by the high R2 parameter (equal to 0.92) of the linear regression trend. The straight interpolating line shows a progressive

1.0 0.9 0.8 0.7

max / UT [MPa]

0.6 0.5 0.4 0.3 0.2 0.1 0.0 1.E+00

BV BE BV run-out BE run-out BF GF CF Possible second linear slope

1.E+02

1.E+04

1.E+06

1.E+08

Nf [cycles]
Fig. 13. Normalised rNf diagram for basalt composites.

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C. Colombo et al. / Composite Structures 94 (2012) 11651174 [4] Landucci G, Rossi F, Nicolella C, Zanelli S. Design and testing of innovative materials for passive re protection. Fire Safe J 2009;44:1103. [5] www.basaltnet.it. [6] Kogan FM, Nikitina OV. Solubility of chrysotile asbestos and basalt bers in relation to their brogenic and carcinogenic action. Environ Health Perspect 1994;102:205. [7] Italian Ministerial Decree D.M. 16.02.1997 Criteri per lomologazione dei prodotti sostitutivi dellamianto. [8] Swink M. Continuous lament basalt. In: Proceedings of techtextil North America symposium, April 2002, Atlanta, GA, USA; 2002. [9] Burgoyne CJ, Taranu N, Pilakoutas K, Serbescu A, Tamuzs V, Weber A. FRP reinforcement in RC structures. FIB technical report. Stuttgart: Sprint Digital Druck Editor; 2007. [10] Van de Velde K, Kiekens P, Van Langenhove L. Basalt bres as reinforcement for composites. In: Proceedings of 10th international conference on composites/ nano engineering, New Orleans, LA, USA; 2026 July 2003. [11] Wu Z, Wang X, Iwashita K, Sasaki T, Hamaguchi Y. Tensile fatigue behaviour of FRP and hybrid FRP sheets. Composites: Part B 2010;41:396. [12] Emery TR, Dulieu-Barton JM. Thermoelastic stress analysis of damage mechanisms in composite materials. Composites: Part A 2010;41:1729. [13] La Rosa G, Risitano A. Thermographic methodology for rapid determination of the fatigue limit of materials and mechanical components. Int J Fatigue 2000;22:65. [14] www.basaltex.com. [15] ASTM D 3039/D 3039M 08, Standard test method for tensile properties of polymer matrix composite materials. [16] ASTM D 3410/D 3410M 95, Standard test method for compressive properties of polymer matrix composite materials with unsupported gage. [17] ASTM D 5528 01 (Reapproved 2007), Standard test method for mode i interlaminar fracture toughness of unidirectional ber-reinforced polymer matrix composites. [18] ASTM D 3479/D 3479M 96 (reapproved 2007), standard test method for tensiontension fatigue of polymer matrix composite materials section by shear loading. [19] www.ir.com. [20] Risitano A, Risitano G, Clienti C. Fatigue limit by thermal analysis of specimen surface in mono axial traction test. In: EPJ web of conferences, vol. 6; 2010. p. 38010, doi: 10.1051/epjconf/20100638010. [21] Greene RJ, Patterson EA, Rowlands RE. Thermoelastic stress analysis. In: Sharpe Jr WN, Sharpe WN, editors. Springer Handbook of experimental solid mechanics; 2008. p. 74767. [22] Clienti C, Fargione G, La Rosa G, Risitano A, Risitano G. A rst approach to the analysis of fatigue parameters by thermal variations in static tests on plastics. Eng Fract Mech 2010;77:2158. [23] Harris B. Fatigue in composites. Cambridge: Woodhead Publishing; 2003. [24] Brmond P, Potet P. Lock-in thermography: a tool to analyze and locate thermomechanical mechanisms in materials and structures. In: Rozlosnik Andres E, Dinwiddie Ralph B, editors. Proceedings of SPIE, thermosense XXIII, vol. 4360, p. 5606. [25] Colombo C, Vergani L. Multi-axial fatigue life estimation of unidirectional GFRP composite. Int J Fatigue 2011;33:1032. [26] Reis PNB, Ferreira JAM, Costa JDM, Richardson MOW. Fatigue life evaluation for carbon/epoxy laminate composites under constant and variable block loading. Compos Sci Technol 2009;69:154.

tests and fatigue tests were carried out. From the obtained results it is possible to propose the following conclusions: basalt reinforced epoxy composites evidenced higher mechanical properties with respect to vinylester, both in the tensile and compressive behaviour, and the failure mode is more compact, since bres do not tend to explode; for both the considered matrices, experimental results are repeatable and evidenced a very low scatter, despite the manual manufacture of the panels; considering fatigue curves in the normalised rmax/rUT Nf plot, a general linear trend for basalt composites was detected; these data can also probably be tted by a double linear interpolation; together with mechanical results, also thermally monitored tests were presented, both static and stepwise for the basaltepoxy composite. From static trend it is possible to detect the stress level at the end of thermoelasticity, while from stepwise thermal analysis two techniques, thermal (DTmean/DN rmax plot) and energetic (D-mode), are considered to monitor variations in the composite behaviour; the transition point between the two linear trends in the rmax/ rUT Nf plot was found to correspond to the evaluated stress level rD. This shows that thermography is a powerful tool to rapidly determine fatigue behaviour of composites.

Acknowledgements Authors would like to thank Prof. Antonio Salerno for his helpful assistance during experimental thermographic tests. A special thanks also to formerly master student Giorgia Gobbi for the panels preparation and help in the experimental tests. References
[1] Czigany T. Discontinuous basalt ber-reinforced hybrid composites (in: polymer composites from nano- to macro-scale). New York: Springer; 2005 [chapter 17, Part IV, 309]. [2] Ross A. Basalt bers: alternative to glass? Compos Technol 2006(August):1. [3] Bashtannik PI, Ovcharenko VG, Boot, Yu A. Effect of combined extrusion parameters of mechanical properties of basalt ber-reinforced plastics based on polypropylene. Mech Compos Mater 1997;33:600.