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Static and dynamical behaviour of mineral fiber reinforced composites with polypropylene matrix

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STATIC AND DYNAMIC MECHANICAL BEHAVIOUR OF MINERAL FIBER REINFORCED COMPOSITES WITH

POLYPROPYLENE MATRIX

P. Tamás

MSc student, Department of Polymer Engineering, Budapest University of Technology and Economics, H-1111 Budapest, Műegyetem rkp. 3., Hungary, e-mail: tcpc19@gmail.com

T. Czigány

Professor, Department of Polymer Engineering, Budapest University of Technology and Economics, H-1111 Budapest, Műegyetem rkp. 3., Hungary, e-mail: czigany@eik.bme.hu

Abstract: Static and dynamic mechanical properties and microstructure of different basalt, carbon and glass fiber reinforced polypropylene composites have been investigated.

Mechanical tests were performed at three different fiber contents. Static mechanical properties were determined with tensile and flexural test, dynamic mechanical properties with falling weight test, microstructure of composites was analyzed with scanning electron microscope (SEM). The results of investigations revealed that the mechanical properties of continuous basalt fiber reinforced composites are better than short basalt fiber reinforced materials. It can be concluded that continuous basalt fibers are competitive with glass fibers.

Keywords: Mineral fiber, Polypropylene matrix, Mechanical properties,

INTRODUCTION

In the last two decades basalt fibers have come into consideration as potential reinforcement of composite materials. Basalt is a common volcanic rock that can be found in most countries around the globe and is directly suitable for fiber manufacturing. Its chemical structure is nearly related to glass. Basalt rocks are molten approximately between 1350 and 1700°C [1-3]. When cooled rapidly, basalt solidifies in a glassy amorphous phase. Slower cooling results a partially crystalline structure, an assembly of minerals. Basalt fibers are good electric insulators, biologically inactive and environmentally friendly. The average density of basalt is 2.7 g/cm3, while glass has a density of 2.5-2.6 g/cm3 [4, 5].

The color of basalt ranges from brown and gray to dull green depending on the chemical composition. Basalt fibers are more resistant to strong alkalis than glass fibers, but glass can withstand better acids. Basalt products can be used over a wide range of temperature, from - 200°C to +600°C [6-8].

Basalt fibers are produced in one step, directly from crushed basalt stone. Basalt fibers can be divided into 2 groups: short and continuous fibers. Some melt blowing technologies (e.g. Junkers method) are suitable for producing cheap, short basalt fibers, but such fibers have relatively poor and uneven mechanical properties. In melt blowing technologies the molten basalt rock is poured onto an ensemble of rotating steel cylinders. As the melt is blown off from the cylinders by air jets, fibers are formed in the air blast and solidify quickly in a glassy amorphous phase. The characteristics of Junkers technology cause the formation of the so-called fiber heads. While some of them break from the fibers, the others - mostly the smaller ones - remain on the fiber ends [9]. Continuous basalt fibers are made by spinneret

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method, similarly to glass fibers (Fig. 1.). The broken basalt stone is molten in a rhodium- platinum pot, lead to a spinneret made from the same material and spun gravitationally through holes in the spinneret bottom at 1350-1420°C. In glass fiber manufacturing mainly overhead gas burners are used for heating the melt. In case of basalt it causes difficulties because due to its dark color it absorbs infrared energy near to the surface, thus homogeneous heating is difficult. This can be overcome by holding the melt in the reservoir for longer time or by electric heating using electrodes immersed in the bath. Basalt stone is molten in two steps: in the initial furnace it is fused, then conveyed to the secondary heating zone feeding the extrusion bushings, equipped with a precise temperature control system [8, 10].

Fig. 1. A simplified sketch of a basalt fiberization processing line: 1) crushed stone silo;

2) loading station; 3) transport system, 4) batch charging station, 5) initial melt zone, 6) secondary heat zone with precise temperature control, 7) filament forming bushings, 8) sizing

applicator, 9) strand formation station, 10) fiber tensioning station, 11) automated winding station

The idea of using basalt fibers as reinforcement of composite materials first emerged in the former Soviet Union in an aerospace research program. Today most of the continuous basalt fibers are manufactured in Russia and Ukraine [8].

The aim of this study was to compare the mechanical properties and fiber-matrix interfacial adhesion of different basalt and other fiber reinforced polypropylene composites.

MATERIALS AND METHODS

Polypropylene fiber was utilized as matrix material, reinforcing material was short (made by Junkers method) and continuous basalt fiber, carbon fiber and glass fiber. Tab. 1.

shows the type and manufacturers of composite raw materials. Short basalt fibers are produced in bulk, while continuous basalt, glass and carbon fibers are prepared in rovings.

The composite plates were prepared in 4 steps (Fig. 2.) [11]. Glass, carbon and continuous basalt fibers were chopped to a length of 60 mm for carding. PP fibers that served as the matrix material and acted also as carrying fibers (BEFAMA 3K type multi-cylinder carding machine) were fed in the machine together with the reinforcing fibers.

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Marking Type of fiber Manufacturer

SBF Short basalt fiber Toplan Ltd., Hungary BF1 Continuous basalt fiber Dnipropetrovsk State

University, Ukraine BF2 Continuous basalt fiber Kamenny Vek Co., Russia CF Carbon fiber Zoltek Co., Hungary GF E glass fiber Skoplast Ltd., Slovakia PP Polypropylene fiber TVK Co., Hungary

Tab. 1. Raw material of tested composites

The carded pre-fabricates were needle punched and as a result became more consistent and contained less air inclusions. 3 mm thick plates were produced from the materials prepared in the way mentioned above with pressing on a Schwabenthan Polystat 300S type pressing machine, at the temperature of 200°C and pressure of 20 bar.

Fig. 2. Production of composite plates [11]

Static mechanical properties of composites were investigated by tensile and flexural tests. Specimens with different dimension were cut from the composite plates (Fig. 3.). Every test was executed in direction of fibers (i.e. direction of carding) and perpendicular to fiber direction with different fiber contents: 10, 20 and 30 mass percentage (m%) in case of continuous basalt fibers and 30 m% in case of other fibers.

Tensile tests were executed according to the EN ISO 527:1999 standard, with 110 mm gauge length on a Zwick Z050 testing machine supplemented with video extensometer, at ambient temperature. The test speed was v=2 mm/min. Flexural tests were executed according to the EN ISO 14125:1999 standard, with 48 mm span length on a Zwick Z020 testing machine, at ambient temperature. The test speed was v=2 mm/min. 5 specimens of each material were tested and mean values and standard deviations were calculated.

Fiber feeding Carding

Needle punching Pressing

Cutting

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a) b) c)

Fig. 3. Composite specimens with different dimension, a) flexural specimen, b) tensile specimen, c) falling weight specimen

Dynamic mechanical properties were investigated by falling weight tests, with 8.26 kg weight and 20 mm spear diameter, on a CEAST Fractovis 6785 instrument, at ambient temperature. The impact speed was v=5 m/s. Ductility index (Dr ) and perforation energy (Ep ) were calculated with the following equations (Eq. 1-2. ) [12]:

− ⋅100

=

max F max

r E

E

D E max [%] (1)

B

Ep = Emax (2)

where EFmax is energy at highest force, Emax is highest energy and B is thickness of specimen.

SEM micrographs of tensile specimen fracture surfaces were made with a Jeol JSM- 5400 scanning electron microscope.

RESULTS AND DISCUSSION

At first the real fiber contents were determined with calcination test. The theoretical and real fiber contents of investigated composites can be seen in Tab. 2.

BF1 BF1 BF1 BF2 BF2 BF2 Theoretical

fibercontent

[m%] 10 20 30 10 20 30

Real fibercontent

[m%] 9.76±1.35 19.42±1.05 29.16±0.91 7.94±1.05 18.80±0.76 27.31±1.18

SBF GF CF

Theoretical fibercontent

[m%] 30 30 30

Real fibercontent

[m%] 17.02±1.14 25.89±1.56 29.92±0.96

Tab. 2. The theoretical and the real fiber contents of investigated composites

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Insignificant difference can be seen between the theoretical and real fiber contents in case of continuous basalt, carbon and glass fibers while a large amount of short basalt fibers fell out during carding.

Letter C indicates specimens with the direction of carding collateral with loading, while P indicates specimens with the direction of carding perpendicular with the direction of loading.

The results of tensile tests were represented in Tab. 4. and Fig. 4-5., the markings can be seen in Tab. 3.

Material BF1

10m% BF1

20m% BF1

30m% BF2

10m% BF2

20m% BF2

30m% PP SBF

30m% GF

30m% CF 30m%

Mark 1 2 3 4 5 6 7 8 9 10

Tab. 3. Marking of investigated materials

BF1 10m%c BF1 20m%c BF1 30m%c BF2 10m%c BF2 20m%c BF2 30m%c σm [MPa] 39.19±1.04 57.33±3.44 67.88±1.57 45.7±1.69 46.71±4.14 47.43±5.13 Em [GPa] 2.67±0.99 4.23±1.86 6.15±1.17 3.07±0.84 2.93±0.87 5.30±1.33

BF1 10m%p BF1 20m%p BF1 30m%p BF2 10m%p BF2 20m%p BF2 30m%p σm [MPa] 30.57±1.89 41.65±0.42 43.5±3.79 31.34±1.02 29.05±1.28 39.87±3.39 Em [GPa] 1.49±0.23 3.35±1.00 3.27±0.71 2.65±0.63 3.05±0.86 3.17±0.76

PPc SBF 30m%c GF 30m%c CF 30m%c

σm [MPa] 28.6±0.30 30.8±0.70 98.4±6.20 84.3±7.10 Em [GPa] 1.318±0.07 1.900±0.11 4.642±0.21 5.164±0.50

PPp SBF 30m%p GF 30m%p CF 30m%p

σm [MPa] 28.6±0.30 28.5±0.60 44.5±1.90 67.2±6.90 Em [GPa] 1.318±0.07 1.762±0.05 2.393±0.05 4.820±0.32

Tab. 4. Results of tensile test (tensile strength: σm, elasticity modulus: Em)

The results show that the tensile properties of continuous basalt fiber reinforced composites can be compared with the glass fiber reinforced composites. The tensile strength of continuous basalt fiber reinforced composites is higher than the tensile strength of short basalt fiber reinforced composites at 30 m% fiber content.

Carding direction

0 20 40 60 80 100 120

1 2 3 4 5 6 7 8 9 10

Material σm [MPa]

Perpendicular direction

0 20 40 60 80 100 120

1 2 3 4 5 6 7 8 9 10

Material

σm [MPa]

Fig. 4. Tensile strength of investigated composites

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Carding direction

0 1 2 3 4 5 6 7 8

1 2 3 4 5 6 7 8 9 10

Material

Em [GPa]

Perpendicular direction

0 1 2 3 4 5 6 7 8

1 2 3 4 5 6 7 8 9 10

Material

Em [GPa]

Fig. 5. Elasticity modulus of investigated composites The results of flexural test can be seen in Tab. 5.

BF1 10m%c BF1

20m%c BF1

30m%c BF2

10m%c BF2

20m%c BF2 30m%c σh [MPa] 56.29±17.32 112.28±0.46 174.25±18.20 78.49±8.72 91.34±4.82 149.99±13.92 Eh [GPa] 1.87±0.41 4.67±0.32 7.25±0.89 2.09±0.72 3.38±0.17 6.57±0.21 BF1

10m%p BF1

20m%p BF1

30m%p BF2

10m%p BF2

20m%p BF2 30m%p σh [MPa] 54.89±1.13 94.26±1.54 107.85±6.08 57.17±5.68 54.67±1.70 103.98±3.82 Eh [GPa] 2.05±0.26 3.7±0.27 4.50±0.13 2.20±0.75 2.18±0.40 4.28±0.56

PPsz SBF 30m%sz GF 30m%sz CF 30m%sz σh [MPa] 38.20±1.00 51.70±3.40 133.40±6.40 146.80±3.70

Eh[GPa] 1.48±0.11 2.46±0.25 4.16±0.31 7.72±0.70 PPk SBF 30m%k GF 30m%k CF 30m%k

σh [MPa] 38.20±1.00 49.00±3.20 67.10±3.00 107.40±9.90

Eh[GPa] 1.48±0.11 2.25±0.21 2.81±0.27 5.84±0.61

Tab. 5. Results of flexural tests (flexural strength: σh, flexural modulus: Eh)

The results show that the flexural properties of continuous basalt fiber reinforced composites can be compared with glass and carbon fiber reinforced composites. The flexural strength of continous basalt fiber reinforced composites is higher than the flexural strengths of short basalt fiber reinforced composites at 30 m% fiber content. The results of flexural tests are shown in Fig. 6-7, the marking can be seen in Tab. 3.

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Carding direction

0 50 100 150 200 250

1 2 3 4 5 6 7 8 9 10

Material σh [MPa]

Perpendicular direction

0 50 100 150 200 250

1 2 3 4 5 6 7 8 9 10

Material

σh [MPa]

Fig. 6. Flexural strength of investigated composites

Carding direction

0 2 4 6 8 10

1 2 3 4 5 6 7 8 9 10

Material

Eh [GPa]

Perpendicular direction

0 2 4 6 8 10

1 2 3 4 5 6 7 8 9 10

Material

Eh [GPa]

Fig. 7. Flexural modulus of investigated composites The calculated values of falling weight tests can be seen in Tab. 6.

BF1 10m% BF1 20m% BF1 30m% BF2 10m% BF2 20m% BF2 30m%

Dr [%] 26.49±1.74 42.37±4.83 59.47±1.01 7.41±2.75 34.32±7.96 59.24±1.97 Ep [J/mm] 2.45±0.15 8.64±1.43 14.89±1.94 2.81±0.34 4.52±0.43 11.60±1.77

PP SBF 30m% GF 30m% CF 30m%

Dr [%] 17.30±1.10 43.00±4.60 59.20±4.00 58.30±6.50 Ep [J/mm] 0.90±0.10 2.40±0.30 7.70±0.70 5.70±0.60

Tab. 6. Results of falling weight tests (Dr ductility index, Ep perforation energy)

The ductility index and perforation energy of continuous basalt fiber reinforced composites was higher than the glass and carbon fiber reinforced composites at 30 m% fiber content. The perforation energy of falling weight tests is represented in Fig. 8., the marking can be seen in Tab. 3.

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0 2 4 6 8 10 12 14 16 18

1 2 3 4 5 6 7 8 9 10

Material

Ep [J/mm]

Fig. 8. Perforation energy of falling weight tests

The ductility index and perforation energy are independent from fiber direction.

The fracture surface of continuous basalt fiber reinforced tensile samples was investigated by scanning electron microscope (Fig. 9.). It can be clearly seen that continuous basalt fibers adhere poorly to the non-polar PP matrix

Fig. 9. SEM micrographs of fracture surfaces of continuous basalt fiber reinforced composites

CONCLUSION

The mechanical properties of basalt, glass and carbon fiber reinforced polypropylene composites have been investigated by tensile, flexural and falling weight tests, the fiber- matrix adhesion was investigated by scanning electron microscope (SEM) analysis. The basalt fibers represented two different production technologies: short basalt fibers made by melt blowing (Junkers method) and continuous basalt fibers made by spinneret method.

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The results of investigations show the mechanical properties of continuous basalt fiber reinforced composites are better than the short basalt fiber reinforced composites. Mechanical properties of continuous basalt fiber reinforced composites are similar to mechanical properties of glass fiber reinforced composites and in some cases approach the mechanical properties of carbon fiber reinforced composites. The interfacial adhesion between the continuous basalt fiber and the polypropylene matrix is very weak. On the basis of investigation it can be concluded that continuous basalt fibers are competitive with glass fibers and short basalt fibers are weaker in terms of quality and mechanical properties.

ACKNOWLEDGEMENTS

Kamenny Vek (Russia) and Toplan Ltd. (Hungary) are kindly acknowledged for the provision of basalt fibers. This work was supported by Jedlik Ányos Programme of Ministry of Economy and Transport of Hungary (ENGPL_07), Hungarian Scientific Research Fund (OTKA K61424) and Hungarian-Czech Science and Technology Programme (TéT CZ-1/08).

REFERENCES

[1] Militky J, Kovacic V, Rubnerová J. Influence of thermal treatment on tensile failure of basalt fibers. Engineering Fracture Mechanics 2002; 69. 1025-33.

[2] Botev M, Betchev A, Bikiaris D. Mechanical properties and viscoelastic behavior of basalt fiber reinforced polypropylene. Journal of Applied Polymer Science 1999; 74.

523-31.

[3] Vas LM, Czigány T. Strength modeling of two-component hybrid fiber composites in case of simultaneous fiber failures. Journal of Composites Materials 2006; 40. 1735- 62.

[4] Keszei S, Matkó Sz, Bertalan Gy. Progress in interface modifications: from

compatibilization to adaptive and smart interphases. European Polymer Journal 2005;

41. 697-705.

[5] Czigány T. Special manufacturing and characteristics of basalt fiber reinforced polypropylene composites: Mechanical properties and acoustic emission study.

Composites Science and Technology 2006; 66. 3210-20.

[6] Morozov NN, Bakunov VS, Morozov EN. Materials based on basalt from the European north of Russia. Glass and Ceramics 2001; 58. 100-4.

[7] Sim J, Park C, Moon DY. Characteristics of basalt fiber as a strengthening material for concrete structures. Composites Part B 2005; 36. 504-12.

[8] Fourné F, Synthetic Fibers. München: Carl Hanser Verlag 1999.

[9] Vas LM, Pölöskei K, Felhős D, Deák T, Czigány T. Theoretical and experimental study of the effect of fiber heads on the mechanical properties of non-continuous basalt fiber reinforced composites. Express Polymer Letters 2007; 1. 109-21.

[10] Gur’ev VV. Neproshin EI, Mostovoi GE. The effect of basalt fiber production technology on mechanical properties of fiber. Glass and Ceramics 2001; 58. 62-5.

[11] Czigány T. Discontinuous Basalt Fiber-Reinforced Hybrid Polymer Composites in:

Polymer Composites: From Nano to Macro-Scale, K. Friedrich (Ed.). München:

Springer Verlag 2005; 309-28.

[12] Liu TM, Baker WE. Instrumented dart impact evaluation of linear low density polyethylene at controlled impact energy. Polymer Engineering and Science 1991;

31. 753-63.

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