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Characterisation and study of the creep behaviour of Polypropylene/Calcium

Carbonate nanocomposites

Article · November 2010

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Journal of Applied Sciences Research, 6(11): 1620-1626, 2010
© 2010, INSInet Publication

Characterisation and Study of the Creep Behaviour of Polypropylene/ Calcium

Carbonate Nanocomposites
1
Mgbemena Chinedum Ogonna, 2Mgbemena Chika Edith, 3Ubani Nelson Obinna
1
Department of Mechanical Engineering, Nnamdi Azikiwe University, Awka- Nigeria.
2
Department of Industrial and Production Engineering, Nnamdi Azikiwe University, Awka- Nigeria.
3
Department of Mechanical Engineering, Michael Okpara University of Agriculture Umudike,
Umuahia- Nigeria.

Abstract: The creep behavior of Polypropylene/Calcium Carbonate nanocomposite were investigated by

conducting creep tests on replicated samples of Polypropylene/Calcium Carbonate nanocomposite at
different loadings of Calcium carbonate (0%,5%,10% and 15%) by varying the Stresses and Temperatures.
It was seen that the resistance to creep was high for the nanocomposite as compared to the unreinforced
Polypropylene. The Creep behavior of the polymer nanocomposite formed was observed to increase with
increase in temperature and stress while the Creep Modulus obtained decreases with increase in time and
temperature. The Creep modulus is steeper at low stress levels.

Key words: Creep, Polypropylene, Calcium Carbonate, Nanocomposite, Creep Modulus

INTRODUCTION curve is shown in figure 1.

The main characteristic of a polymer creep process
(far from rupture) is a progressive strain increase at a
decreasing rate, until this rate reaches either a constant
(under viscous flow) or a zero value (for cross-linked
amorphous or semi-crystalline polymers). Creep is a
time- and temperature-dependent phenomenon,
occurring under load control. In creep, the material’s
temperature is a governing factor regarding what
happens. However, some creep may occur even at low
homologous temperatures, and they are not always
negligible. For polymers, the creep regime is above the
glass transition temperature. Creep appears to be
combinations of behaviors of viscous liquids and elastic
solids[1].
Plastics also creep at ambient temperatures but,
compared to lead, they are able to sustain much greater
extensions before failure, the creep curves are similar
in shape to those for metals, but the mechanism of
deformation is quite different because of the difference
in structure of the material[1,8].
A polymer consists of long chain-like molecules in
a tangled and coiled arrangement; creep occurs by
chains untangling and slipping relative to one another.
The creep rate is dependent on stress and temperature.
A creep test is carried out by applying a constant
load to a specimen and observing the increase in strain
(or extension) with time. A typical extension - time
Three regions can be readily identified on the
curve:
Stage I Primary Creep – the creep proceeds at a
diminishing rate due to work hardening.
Stage II Secondary Creep – the creep proceeds at a
constant rate because a balance is achieved
between the work hardening and annealing
(thermal softening) processes.
Stage III Tertiary Creep - the creep rate increases due
to necking and the associated increase in
local stress of the specimen. Failure occurs at
point 4.
In terms of dislocation theory, dislocations are
being generated continuously in the primary stage of
creep. With increasing time, more and more
dislocations are present and they produce increasing
interference with each other’s movement, thus causing
the creep rate to decrease. This dynamic equilibrium
causes the material to creep at a constant rate.
However, the creep rate increases and the specimen
fails due to localized necking of the specimen (or
component), void and micro crack formation at the
grain boundaries, and various metallurgical effects such
as coarsening of precipitates.
When in service, an engineering component should
never enter the tertiary stage of creep. It is therefore
the secondary creep stage, which is of prime

Corresponding Author: Mgbemena Chinedum Ogonna, Department of Mechanical Engineering, Nnamdi Azikiwe University,
Awka- Nigeria.
E-mail: edumgbemena@yahoo.com Phone: +2347034308877
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 J. Appl. Sci. Res., 6(11): 1620-1626, 2010
importance as a design criterion. Components, which
are subject to creep, spend most of their lives in the
secondary stage, so it follows that the metals, alloys
and plastics chosen for such components should have
as small a secondary creep rate as possible[3,5,6,8].
In general it is the secondary creep which
determines the life of a given component. Secondary
creep for a particular metal, alloy or plastic depends on
several variables, the most important of which are
stress and temperature. The most commonly used
expression for relating secondary creep rate ε to stress
σ and absolute temperature T has the form
E
  A e n RT
(1)
Where A and n are constants, E is the activation
energy for creep in the metal and R is the universal
gas constant (8.31 J/mol K)[5].
The equation shows that the creep rate is increased
by raising either the stress or the temperature. Taking
natural logarithms gives:
ln ε = ln A + n ln σ - E/T (2)
Thus, for tests at constant temperature and varying
stress, the stress exponent n can be found by plotting
ln ε against ln σ alternatively, if the stress is kept
constant and the temperature varied, E can be
determined by plotting In ε against l/T.
The fact that the exponent n varies with stress
demonstrates the inadequacy of simple laws for
correlation of data over a wide range of stress levels.
In practice, more complicated equations are used to
correlate experimental data.
2.0 Experimental:
2.1 Materials and Sample Preparation: The PP was
melted from its pelletized form at a temperature
exceeding 1800C in a mixing chamber. Measured
amounts of Calcium Carbonate were added to the
melted PP by volume fractions and stirred continuously
for 10 minutes to ensure a uniform dispersion of the
mixture. The compounded mixture was cast in an
aluminum mould that has been treated with a mould
releasing agent and dried. The composite was allowed
to cure and was later de-moulded. The above procedure
was repeated for the stearic acid coated Calcium
Carbonate previously done (i.e. at 0%, 5%, 10%, and
15% volume fractions). The fabricated material has a
dimension of 85mm x 35mm x 10mm[8].
2.2 The Creep Test: The creep measurements were
carried out with a SM106 MK II Creep Testing
Machine. The strain/force vs. time experimental data
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was recorded. The test specimens were previously
conditioned at 25oC, and the creep tests were
conducted at each selected temperature (i.e. at 25, 50
and 70 o C) in a thermostatic chamber under applied
stresses of 13.08, 19.60, and 22.87 MPa for three
different volume fractions of stearic acid coated
Polypropylene/Calcium carbonate nanocomposites and
neat Polypropylene[3,8].
RESULTS AND DISCUSSIONS
For each volume fraction, six samples were tested.
Plots were made to show the relationship between i)
Elongation vs. Time, ii) Creep Modulus vs. Time and
iii) ε vs. t were made. Tests were conducted at
different loads and stresses.
The creep experiment was performed using the
coated CaCO3 fillers initially at an ambient temperature
of 25oC varying the stresses at 13.08MPa, 19.60MPa
and 22.87MPa; then at the following temperatures:
50oC and 70oC.In all the temperatures, the creep
response were non-linear.
From figures 3, 5, 7, 9 and 11, it was found that
creep increases with temperature and stress. Creep is
more severe and faster with materials subjected to heat
for long periods. This is largely due to the fact that
stress decreases the activation barrier for bond
dissociation, thus allowing the molecular chains to
move more easily; with increasing tensile stress, the
movement of the molecular chains increases rapidly
and creep is accelerated. Also from figures 4, 6, 8, 10,
and 12 the Creep Modulus obtained decreases with
increase in time and temperature. It is steeper at low
stress levels.
Creep and Creep fracture represents one of the
major problems associated with the selection and use
of engineering materials for high temperature
applications. Poor creep resistance and dimensional
stability of thermoplastics is generally a deficiency,
impairing the service life and safety which is a barrier
for further expansion in engineering. Resistance to
creep is very high for nanocomposites compared to
neat Polypropylene matrix because calcium carbonate
resists the slippage, re-orientation and motion of the
polymer chain in the nanocomposite. From the
foregoing, it is clear that the strength of a nano-filled
composite depends to a great extent on the interfacial
adhesion between the polymer matrix and the nano-
filler which aids the transfer of a small section of
stress to the filler particle during deformation. The
creep rupture is a function of Temperature.
 J. Appl. Sci. Res., 6(11): 1620-1626, 2010

Fig. 1: A Typical Creep Curve[1].

Fig. 2: Relationship between creep rate and total strain on a log-log scale[1].

Fig. 3: Comparative Creep Response for PP/CaCO3 at 13.08MPa (ambient temperature of 25EC).

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 J. Appl. Sci. Res., 6(11): 1620-1626, 2010

Fig. 4: Creep Modulus vs. Time for PP/CaCO3 at 13.08MPa and ambient temperature of 25EC.

Fig. 5: Comparative Creep Response for PP/CaCO3 at 19.60MPa and ambient temperature of 25EC.

Fig. 6: Creep Modulus vs. Time for stress of 19.60MPa and ambient temperature of 25EC.

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 J. Appl. Sci. Res., 6(11): 1620-1626, 2010

Fig. 7: Comparative Creep Response at 22.87MPa and ambient temperature of 25EC.

Fig. 8: Creep Modulus vs. Time for a stress of 22.87MPa and ambient temperature of 25EC.

Fig. 9: Comparative Creep Response at Temperature of 50oC and stress of 13.08MPa

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 J. Appl. Sci. Res., 6(11): 1620-1626, 2010

Fig. 10: Creep Modulus vs. Time for a Temperature of 50oC

Fig. 11: Comparative Creep Response at Temperature of 70oC and stress of 13.08MPa

Fig. 12: Creep Modulus vs. Time for a Temperature of 70oC

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 J. Appl. Sci. Res., 6(11): 1620-1626, 2010
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Master of Engineering thesis, Department of
Mechanical Engineering, Blekinge Institute of
Technology, Karlskrona, Sweden.
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5. Dieter, G.E., 1988 ”Mechanical Metallurgy”, I
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