Chapter 1

Mechanical and Tribological Properties of Scrap Rubber Based

Composites Reinforced with Glass Fiber, Al and TiO2

L.M.P. Ferreira, I. Miskioglu, E. Bayraktar, and D. Katundi

Abstract Scrap rubber/Epoxy composites reinforced with Aluminium, Glass Fibre (GF) and TiO2 particles were prepared
and mechanical and tribological properties of these composites were investigated. Basically, these composites are aimed to
use in automotive and aeronautics applications. A detail microstructure and matrix/reinforcement interface analyze was
made by means of Scanning Electron Microscope (SEM) The wear performance of hard particles reinforced composites
were evaluated. Quasi static and dynamic compression tests were carried out and damaged specimens were studied by SEM.
The hardness (short test) values of the composites were reviewed related to the reinforcement elements, Glass Fibre-fiber
and TiO2 added in the matrix.

Keywords Recycling materials • Rubber/epoxy composites • Low-cost engineering • Wear resistance

1.1 Introduction

In engineering applications, there are many possibilities for usage of recycling of scrap rubber and most of them are used in
automotive industry and domestic area, etc. Other main areas such as the aerospace and microelectronics industries have
enourmous demand for high performance (ductile and high toughness) structural adhesive systems like epoxy and/or
elastomers reinforced composites [1–9]. Today, additionally, the main component of these waste rubbers is styrene–
butadiene rubber (SBR) and, in spite of the different uses for recycling it, the research for new applications is still a need
because of the extremely high amount of waste rubber produced every year [5–8, 10–16].
Additionally, these materials are commonly used for long term applications at ambient or at moderately elevated
temperature conditions. Conforming to these needs, elastomers (rubbers) should be used by simple processing with various
materials in different conditions by addition of new alloying elements [7–11].
The present work reviews manufacturing facilities of scrap elastomers (SBR-rubbers) + epoxy resin composites with
different proportions of particulate reinforcements. Main objective of this research was to determine the ductility and
toughness of scrap elastomer (SBR rubber) matrix composites containing GF, TiO2, B, etc. as basic reinforcements.
Basically, these composites are aimed to use in automotive and aeronautics applications as bumpers and as internal furniture
as ductile and tough and sound materials. Scanning electron microscopy (SEM) was used to study the microstructure and
fracture surfaces of these composites.

L.M.P. Ferreira
Materials Science Department, UNICAMP—University of Campinas, Campinas, São Paulo, Brazil
School of Mechanical and Manufacturing Engineering, Supmeca-Paris, Paris, France
I. Miskioglu
Department of ME-EM, Michigan Technological University, Houghton, MI, USA
E. Bayraktar (*)
School of Mechanical and Manufacturing Engineering, Supmeca-Paris, Paris, France
e-mail: bayraktar@supmeca.fr
D. Katundi
Materials Science Department, UNICAMP—University of Campinas, Campinas, São Paulo, Brazil

# The Society for Experimental Mechanics, Inc. 2017 1

W.C. Ralph et al. (eds.), Mechanics of Composite and Multi-functional Materials, Volume 7,
Conference Proceedings of the Society for Experimental Mechanics Series, DOI 10.1007/978-3-319-41766-0_1

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2 L.M.P. Ferreira et al.

1.2 Experimental Conditions

At the beginning of the composite design, scrap rubber powders were chemically treated by toluene, acrylic acid and
vinyltriethoxysilane (2 %) then dried in an oven to eliminate trace of the chemicals. After chemical treatment, 60 % of scrap
rubber and 40 % of epoxy were mixed used as matrix. TiO2 was chosen as main reinforcing element together; with
aluminum, glass-fiber, as minor reinforcement elements, boron and Cu were also added in the matrix (Table 1.1).
Four basic compositions were prepared after here will be called RETIG-1, 2, 3 and 4.
After preliminary blending of the basic elements (scrap rubber + epoxy) of the composites, reinforcement elements were
added in the structure and entire of the mixture have been milled for 2 h to obtain a homogenous compound. At the final
stage, the specimens were manufactured by hot compacting (double uniaxial action) under a pressure of 70 MPa at the
temperature of 180  C. The dwell time for the compacting process was 15 min. All of the specimens (30 mm diameter, 6 mm
thick) were cooled down slowly. The post curing was concluded under isothermal conditions at 80  C for 48 h. Shore D
hardness test was performed on the polished flat surfaces of the specimens according to ASTM D 2240 using durometer
Shore test device, (type HBD-100-0). Shore D was also performed for the samples exposed to Ultra Violet (UV) conditions
during exposing time: 2 months (every week during months) to evaluate resistance of these composites against degradation
by UV.
Macroindentation test was carried out at room temperature using a stainless steel ball with 3 mm diameter. For this test,
ten specimens for each composition were prepared with diameter of 40 mm. Thickness of the specimens was variable from
6 up to 10 mm. Maximum force (Fmax) at failure and fracture surface were evaluated by SEM analysis.
Again, dynamic compression (drop weight tests) was carried out using a universal drop weight test device, Dynatup
Model 8200 machine, with a total weight of 1.9 kg, punch height of 600 mm and with an impact velocity of around 3 m/s.
Wear resistance were evaluated by nanoindentation tests under two different normal loads (20 and 50 mN) applied over a
linear track of 500 μm for 50 cycles. Wear is performed with a conical tip that has 90 degree apex angle. One cycle is defined
as a pass and return of the tip over the track; the total distance for one test was 0.050 m. The speed of the tip during wear tests
was 50 μm/s. A total of 10 wear test was performed for each sample.

1.3 Results and Discussion

General microstructure of the specimens was presented in the Fig. 1.1 for four compositions. All of the microstructures of the
composites presented here are more and less homogenous. Chemical fusion bonding of rubber with epoxy powders were
made perfectly thanks to the initial chemical treatment of the scrap rubber.
Certain area in the structure shows weakly agglomeration of the reinforcements. This type of agglomeration can be
improved by milling in longer time.
Comparison of hardness (Shore D) results were compared in the Fig. 1.2 for four different compositions after exposing to
ultraviolet (UV) during 7, 14, 21, 28 and 45 days. As seen from this graphics, there is no change significantly on the
measured values for each period. In reality, all of the specimens have kept their original structure any decohesion between
chemical bindings (not chemical deterioration). Addition of boron is always a positive effect on the hardness behaviour of
these composites even if its percentage is very low. However, some small cracks appeared on the thin specimens at the end of
long exposing time (around 2 months). This behaviour is worthy for the pieces aimed on the production of external parts used
for example in the car industry (i.e. bumpers) [7–13]. All of the four composites gave the same level of hardness.

Table 1.1 General compositions of the rubber based composites (RETIG)

Matrix
Rubber 60 %
Compositions Epoxy 40 % Al Glass-fiber TiO2 B Cu
RETIG-1 B 7 7 0 1 1
RETIG-2 B 7 7 7 1 1
RETIG-3 B 7 7 10 1 1
RETIG-4 B 7 7 15 1 1

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Fig. 1.1 General microstructures of the compositions in transversal section

Fig. 1.2 Comparison of

Shore D results for four
different compositions after
exposing to ultraviolet
(UV) during 7, 14, 21, 28
and 45 days

Macroindentation test results were presented in the Fig. 1.3 presented with maximum forces at the failure. A considerable
scattering on the values was found for each composite. This type of the damage analysis is very well-meaning related the
structure of this type of composites. Damaged surfaces obtained from this test were evaluated by SEM (Fig. 1.4).
Fracture surfaces for all of the composites have shown very tough structure without internal defects (porosity, decohesion
of the particulate reinforcements, etc.). Ductility is observed in many parts of the surfaces and increasing from the first
composite (RETIG-1, TiO2 value is 0 %) up to the fourth composite (RETIG-4, TiO2 value is 15 %) these observations are
justified with the results observed from Fig. 1.3.
Another damage analysis has been performed by dynamic compression and/or drop weight test as given the entire test
conditions in the former section (experimental conditions) and absorbed energy were calculated for each composite via “Mat
lab” from the data base (Fig. 1.5).

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Fig. 1.3 Maximum values

(Fmax) obtained for each
composition obtained by
macroindentation test

Fig. 1.4 Fracture surfaces of the samples for the compositions after macroindentation test presented in this work

Fracture surfaces of this test were evaluated in the Fig. 1.6. Again, the glass fibers added in the structure play a role like a
bridge between the matrix and reinforcements. In fact, ductile behaviour of these composites is a combined effect of the
main reinforcement of TiO2 and glass fibers. Even if the slope is weakly incremental, addition of glass fibre together with
TiO2 improves ductility agreement with former papers published in [4, 14, 16]. All of these results obtained by dynamic
compression tests confirmed well former results discussed in the Figs. 1.3 and 1.4.
Wear track deformation by using nanoindentation tests gave much more information on the micromechanical properties
of the composites proposed in this work. Wear resistance were evaluated by nanoindentation tests under two different

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1 Mechanical and Tribological Properties of Scrap Rubber Based Composites Reinforced with Glass Fiber, Al and TiO2 5

Fig. 1.5 Energy and liner tendency as a function of the particulate reinforcements found for four compositions obtained by dynamic
compression test

Fig. 1.6 Fracture surface of the samples taken from four compositions obtained by dynamic compression tests

normal loads (20 and 50 mN) applied over a linear track of 500 μm for 50 cycles. Wear damage was performed with a conical
tip that has 90 degree apex angle. Figure 1.7 presents total results of this evaluation. Each column in the figure gives mean
value of 10 wear tests. One may observed that the wear tracks are not perfectly straight, apparently the conical tip is not
fracturing the hard particles (i.e. boron), and just going around them. Another reason can be attributed to the well adhesion of
the particles that they are not pulled out of the matrix (without debonding, they keep their positions in the matrix). It means
that very good adhesion related to very good interface passage between the particles and the matrix was observed on all of
the compositions.

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6 L.M.P. Ferreira et al.

Fig. 1.7 Comparison of wear

track deformation results
tested on the four
compositions under the loads
of 20 and 50 mN

1.4 Conclusions

In the frame of the common research project going on, four new composites were designed from scrap elastomers (SBR)
matrix powders essentially reinforced with GF, Al, TiO2, B, B, and pretreated with fine epoxy resin. Chemical treatment of
rubber powders with vinyltriethoxysilane gave very successful mixture with epoxy resin resulted by well adhesion bonding
with particulate reinforcements. Experimental results obtained from the four different compositions were discussed in the
present work. Mechanical and tribological properties of these composites were evaluated under different test conditions.
Degradation of the specimens was too low after a long exposure 2 months against UV. Combined effect of TiO2 and glass
fibres gives a ductile behaviour in case of impact (drop weight) damage tests. Homogeneous distribution of the
reinforcements in the matrix can be improved by longer milling time at the beginning of the process.

References

1. Zaimova, D., Bayraktar, E., Katundi, D., Dishovsky, N.: Elastomeric matrix composites: effect of processing conditions on the physical,
mechanical and viscoelastic properties. J. Achiev. Mater. Manuf. Eng. 50(2), 81–91 (2012)
2. Papadopoulos, A.M.: State of the art in thermal insulation materials and aims for future developments. Energy Build. 37, 77–86 (2005)
3. Zaimova, D., Bayraktar, E., Miskioglu, I.: Manufacturing and damage analysis of epoxy resin-reinforced scrap rubber composites for
aeronautical applications. In: Tandon, G.P., Tekalur, S.A., Ralph, C., Sottos, N.R., Blaiszik, B. (eds.) Experimental Mechanics of Composite,
Hybrid, and Multifunctional Materials, vol. 6, pp. 65–76. Springer, New York (2014)
4. Zaimova, D., Bayraktar, E., Miskioglu, I., Katundi, D.: Manufacturing of new elastomeric composites: mechanical properties, chemical and
physical analysis. In: Tandon, G. (ed.) Composite, Hybrid, and Multifunctional Materials, vol. 4, pp. 139–150. Springer, New York (2015)
5. Kaynak, C., Sipahi-Saglam, E., Akovali, G.: A fractographic study on toughening of epoxy resin using ground tyre rubber. Polymer 42,
4393–4399 (2001)
6. Yesilata, B., Turgut, P.: A simple dynamic measurement technique for comparing thermal insulation performances of anisotropic building
materials. Energy Build. 39, 1027–1034 (2007)
7. Bessri, K., Montembault, F., Bayraktar, E., Bathias, C.: Understanding of mechanical behaviour and damage mechanism in elastomers using
X-ray computed tomography at several scales. Int. J. Tomogr. Stat. 14, 29–40 (2010)
8. Bayraktar, E., Antholovich, S., Bathias, C.: Multiscale observation of fatigue behaviour of elastomeric matrix and metal matrix composites by
X-ray tomography. Int. J. Fatigue 28, 1322–1333 (2006)
9. Bayraktar, E., Miskioglu, I., Zaimova, D.: Low-cost production of epoxy matrix composites reinforced with scarp rubber, boron, glass bubbles
and alumina. In: Ralph, C., Silberstein, M., Thakre, P.R., Singh, R. (eds.) Mechanics of Composite and Multifunctional Materials, vol. 7, pp.
163–172. Springer, New York (2015)

lygiamaria@fem.unicamp.br
1 Mechanical and Tribological Properties of Scrap Rubber Based Composites Reinforced with Glass Fiber, Al and TiO2 7

10. Bayraktar, E., Isac, N., Bessri, K., Bathias, C.: Damage mechanisms in natural (NR) and synthetic rubber (SBR): nucleation, growth and
instability of the cavitations. Int. J. Fatigue Fract. Struct. Mater. 31(1), 1–13 (2008)
11. Pacheco-Torgal, F., Ding, Y., Jalali, S.: Properties and durability of concrete containing polymeric wastes (tyre rubber and polyethylene
terephthalate bottles): an overview. Construct. Build Mater. 30, 714–724 (2012)
12. Luong, R., Isac, N., Bayraktar, E.: Damage initiation mechanisms of rubber. J. Arch. Mater. Sci. Eng. 28(1), 19–26 (2007)
13. Zaimova, D., Bayraktar, E., Miskioglu, I., Dishovsky, N.: Optimization and service life prediction of elastomeric based composites used in
manufacturing engineering. In: Tandon, G.P., Tekalur, S.A., Ralph, C., Sottos, N.R., Blaiszik, B. (eds.) Experimental Mechanics of Composite,
Hybrid, and Multifunctional Materials, vol. 6, pp. 157–166. Springer, New York (2014)
14. Zaimova, D., Bayraktar, E., Miskioglu, I.: Characteristics of elastomeric composites reinforced with carbon black and epoxy. In: Ralph, C.,
Silberstein, M., Thakre, P.R., Singh, R. (eds.) Mechanics of Composite and Multifunctional Materials, vol. 7, pp. 191–202. Springer,
New York (2015)
15. Nacif, G.L., Panzera, T.H., Strecker, K., Christoforo, A.L., Paine, K.A.: Investigations on cementitious composites based on rubber particle
waste additions. Mater. Res. 16(2), 259–268 (2013)
16. Zaimova, D., Bayraktar, E., Miskioglu, I., Katundi, D.: Study of influence of SiC and Al2O3 as reinforcement elements in elastomeric matrix
composites. In: Tandon, G. (ed.) Composite, Hybrid, and Multifunctional Materials, vol. 4, pp. 129–138. Springer, New York (2015)

lygiamaria@fem.unicamp.br