6th Asean Microscopy Conference, 10-12 December 2007, Impiana Cherating Hotel, Pahang, Malaysia

FRACTURE TOPOGRAPHY STUDY OF BORON CARBIDE POWDER- RUBBER

COMPOSITE APPLIED IN UNIAXIAL TENSILE LOADING CONDITION

Hafizal Yazid, A. Aziz Mohamed, *Sahrim Ahmad, Mohd B. Harun,

W. Saffiey W. Abdullah, Azali Muhammad
Zaiton Selamat, Zahid Abdullah and Shariff Sattar

Malaysian Nuclear Agency (Nuclear Malaysia),

Bangi, 43000 Kajang, Selangor, Malaysia.

*Universiti Kebangsaan Malaysia (UKM)

Bangi, 43000 Kajang, Selangor, Malaysia.

ABSTRACT

The boronated rubber was subjected to uniaxial tensile loading condition until fracture. It was found
that the filled 10phr boron vulcunizate posses lower tensile strength as compared to unfilled
vulcunizate. The reduction is about 5.8 Mpa. This indicate that the addition of boron carbide powder
act as impurities in the rubber matrix. This is supported by fractography study as the boron carbide
powder was found not to properly bonded to the rubber matrix and in some areas, a gap was found in
between the powder and the rubber matrix. Even the reduction in tensile strength occurred, the
boronated rubber was still suitable for radiation shielding purpose as the boron powder is still
available in the rubber matrix providing not to exceed its maximum tensile strength.

Keywords: Boronated rubber, Tensile strength, Impurities, Fractography

1. Introduction

Rubber are widely used in industries due to its elasticity and deformable characteristics [1].
Some of the product made of rubbers are applied in the nuclear industry. This is the critical industry
where product performance is vital in term of safety. One typical example is the use of natural rubber
composites as radiation shielding materials. Boron carbide powder are added to the rubber compound
to become a composite used as radiation shielding. The boronated rubber composite is also developed
by Nuclear Malaysia and Universiti Kebangsaan Malaysia with the intention to be used in TRIGA
Mark II research reactor. Thus the reliability and the performance of the product also depends on the
failure resistance. A clear understanding of the failure mechanism provides a clue to predicting the
service life of rubber products [2]. In general, fracture studies of polymers are conducted from two
different angles, (i) polymer physics, i.e correlation of various mechanical properties of the components
through mathmatical models, and (ii) by careful examination of the microstructure of the fracture
surface to intepret the failure mechanism [3]. In this paper, the sample are subjected to uniaxial tensile
test until fracture and the fracture surface is examined using scanning electron microscopy (SEM) to
intepret the failure mechanism. Setua et al., [4-9] have made successful attempts in the correlation of
mechanical properties of elastomers and composites with the topography of the failure surfaces
recorded under the SEM. SEM is an ideal way as it provides a topographic image and thus an insight
into the problem since little is known about the damaged zone, where deformation and fracture take
place. Therefore this paper aims at finding the relationship between the fracture features and tensile
strength of the natural rubber and boronated natural rubber composite.

2. Experimental Procedures

The developed material is in the form of sheet with thickness of 2mm. The material composed
mainly of natural rubber and 10 phr of boron carbide powder with an average size of 100 μm. Typical
industrial mixing condition was used in the development of the said natural rubber composite. Natural
rubber, boron carbide powder and other additives were mixed in the internal mixer to form uncured
sample. Then the uncured sample was vulcunized by using a vertical 2-piece heated press at 150ºC and
pressure 5 Mpa for an optimum curing time of T 95. The cure time was determined by a rheometer test.
 6th Asean Microscopy Conference, 10-12 December 2007, Impiana Cherating Hotel, Pahang, Malaysia

The cured sample was then subjected to testing. The same procedure was applied to another set of
rubber compound but without the addition of boron carbide powder. In this paper, the sample are
denoted as natural rubber and boronated natural rubber composite.

A Shore A type durometer was employed to find out the hardness of the vulcunizates. The
method adopted is the same as that of ISO 7619:1997 and the readings were taken after 15 secs of
indentation. Specimens for tensile testing were punched out from the vulcunized sheets along the
milling or the „grain‟ direction. Tensile testing was done as per BS-6746 using dumb-bell specimens as
in Fig. 1a and 1b. The rate of grip separation is 100mm/min. This test also enabled us to measure
elongation at break values. Fractography study was carried out by using scanning electron microscope,
SEM- FEI Quanta 400 model.

Fig. 1a: Schematic diagram of tensile specimen Fig. 1b: Tensile specimen

3. Results and Discussion

Table1: Hardness measurement

No Sample Avarage hardness value, Shore A
1 Natural rubber 48.4 ± 0.2
2 Boronated natural rubber 51.7± 0.3

Physical Properties of Vulcunizates

70

60

50

40

30

20

10

0
NR NR Composite

Elongation at break x 10% Tensile strength (Mpa)

Fig. 2: Physical properties of vulcunizates

 6th Asean Microscopy Conference, 10-12 December 2007, Impiana Cherating Hotel, Pahang, Malaysia

Rough
areas
Smooth
areas

Fig. 3: Fracture surface of Natural Rubber Fig. 4. Fracture surface of Natural Rubber
vulcunizate 32x composite vulcunizate 32x

Tear line

Gap between
boron carbide and
rubber matrix.

Fig. 5: As in Fig. 10 at higher magnification 200x Fig 6: As in Fig. 11 at higher magnification 200x

Holes Holes

Loose particle of
Boron carbide

Fig 7: Natural Rubber composite vulcunizate Fig. 8: Natural Rubber composite vulcunizate
showed present of holes 50x showed present of holes and boron carbide 300x
 6th Asean Microscopy Conference, 10-12 December 2007, Impiana Cherating Hotel, Pahang, Malaysia

Fig. 9: EDX scan area for natural rubber Fig. 10: EDX analysis shows present of main element
vulcunizate, E-SEM Mode 500x of natural rubber vulcunizate namely C, O, Zn and S.

Fig. 11: EDX spot analysis A, for natural rubber Fig. 12: EDX analysis shows present of main element
composite vulcunizate, E-SEM Mode 500x and also with the present of Boron.

Avarage hardness value (Shore A) for natural rubber vulcunizate and natural rubber composite
vulcunizate was 48.4 ± 0.2 and 51.7 ± 0.3 respectively. The increase in hardness value for natural
rubber composite vulcunizate is due to the present of hard boron carbide particles in the rubber matrix
which in turn gives rise to the overall hardness of the sample. This is supported by energy dispersive x-
ray spectroscopy (EDX) analysis which shows the present of Boron with other typical element in the
natural rubber composite vulcunizate. The image of EDX spot area is shown in Fig. 11 and the
spectrum is in Fig. 12. Figs. 9 and 10 show the EDX scan area and the spectrum for natural rubber
vulcunizate respectively. The spectrum shows typical element found in the natural rubber vulcunizate
namely C, O, Zn and S.
Tensile strength was 22.5 Mpa for natural rubber vulcunizate. This value is very close to the
value reported by N. M Mathew et. al. [10] for natural rubber vulcunizate, which is 22.4 Mpa. This is
due to the typical rubber compound formulation for natural rubber vulcunizate was used for both of the
samples. As the boron carbide powder was added to the rubber compound, the tensile strength reduced.
The same trend was reported by V. M. Murthy et. al. [11] that the addition of glass fibre as fillers
lowers the tensile strength values. In the present work, the value for natural rubber composite
vulcunizate is 16.7 Mpa. The reduction is about 5.8 Mpa. This indicates that the boron carbide powder
act as a non-reinforcing nature of filler once incorporated in the natural rubber compound. The same
trend again was reported by N. M Mathew et. al. [10] in the case of clay-filled natural rubber
vulcunizate. The addition of fillers does not enhance the tensile strength appreciably. In our work,
elongation at break value for both natural rubber and natural rubber composite vulcunizate shows the
same trend as the tensile strength. The value reduced from 664% for natural rubber to 582% for the
composite. The reduction in elongation at break is also due to the present of boron carbide in the rubber
matrix.
 6th Asean Microscopy Conference, 10-12 December 2007, Impiana Cherating Hotel, Pahang, Malaysia

Fig. 3 shows fracture surface of natural rubber vulcunizate. The area consists of smooth and
rough areas. There are also several tear lines at the smooth areas. It is clearly seen that the tear lines
originate from the rough areas. This is due to the present of flaws and nicks at the edge in the test
specimen, thus cause stress concentration and failure starts from these points. This evidence is
supported by Gent and Lindley [12] that suggested high stress concentration near the flaws would be
adequate enough to produce cavitation in the rubber of conventional modulus and this may be the cause
of the roughness developed around the tip. Once the failure starts, it proceeds through a catastrophic
tearing giving rise to a comparatively smooth surface with some tear lines. The tear line is clearly seen
in Fig. 5.
Fracture surface of natural rubber composite vulcunizate is shown in Fig. 4 and differ
remarkably from the natural rubber vulcunizate. The surface is rough with a number of random
distributed holes. There were also flaws and nicks present on the surface. A higher magnification of
Fig. 4 reveals the present of gap between the boron carbide powder and the rubber matrix. This is
shown in Fig. 6. The present of holes are also shown in Figs. 7 and 8. A loose boron carbide particle
was clearly observed on the surface as in Fig. 8. The holes which appear on the surface is the result
from the removal of loosely bound boron carbide particles from the matrix during fracture. A similar
phenomenon was observed by N. M Mathew et. al. [10] during tear fracture of clay-filled natural
rubber vulcunizate.
Elastomers are often filled with high loadings of relatively rigid particulate materials in order
to stiffen and strengthen them. These effects depend strongly upon the particle size of the filler and the
degree of bonding between the elastomer and the filler [13]. When the particle size is small, less than
about 1μm, even a moderate degree of interaction between elastomeric matrix and the filler seems to be
sufficient to produce a surprisingly high level of reinforcement. When the particle size is relatively
large, the matrix seems to be easily detached from the filler particles at relatively low tensile stresses
and the level of reinforcement is correspondingly low [13]. In our work, the average size of boron
carbide particle is 100 μm. This agrees well from the previous finding that comparatively large
particles would result in easy detachment of filler from the matrix and thus reduce the tensile strength.
It is common that sample edges, moulding imperfections, dirt particles or impurities and
inhomogeneities in the mixes, are deleterious to the strength peoperties of rubber, these could act as
stress raisers and cause initiation of failure of rubber at these points [14]. The same applies in our case
that the location of boron carbide particles is a weak point in the rubber matrix. The particles behave as
impurities and act as stress raisers in the rubber. Thus degrade the properties of the resulted rubber
composite. In this work, even the rubber composite properties degrade, the role of this sample as
radiation shielding material is still not being affected as the key element of boron carbide particle still
available in the rubber matrix providing the application not to exceed its maximumm tensile strength.

4. Conclusions

Fracture topography of boron carbide-filled natural rubber vulcanizate and natural rubber vulcanizate
differ remarkably. The fracture surface of filled natural rubber consists of smooth and rough areas. The
present of tear lines also was observed in the smooth areas. The fracture surface of un-filled natural
rubber consists of rough areas and a number of random distributed holes. The holes are due to the
detachment of hard boron carbide particles from the rubber matrix during fracture. Poor bonding
between the filler and matrix was found for this type of boron carbide and natural rubber matrix system
as the fracture occured at relatively low tensile stress. Additionally the location of boron carbide
particles is a weak point in the rubber as it contains gap and could be treated as impurities which act as
stress raisers. Thus again reduce the tensile strength of the boron carbide- natural rubber composite.

Acknowledgement

The authors thank Dr Azali Muhamad; Materials Technology Group Manager, Dr Abd. Nassir Ibrahim;
Industrial Technology Divisional Director and other Materials Technology Group staff for supporting
this work.

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 6th Asean Microscopy Conference, 10-12 December 2007, Impiana Cherating Hotel, Pahang, Malaysia

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