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EXPERIMENTAL CREEP TESTS ON CONCRETE MADE WITH

MONTMORILLONITE NANO PARTICLES

Conference Paper · July 2012

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 8th International Conference: Concrete in the Low Carbon Era

Dundee, UK, 9-11 July, 2012

EXPERIMENTAL CREEP TESTS ON CONCRETE MADE WITH

MONTMORILLONITE NANO PARTICLES

A. Sprince, L. Pakrastinsh, A. Korjakins

Abstract. The purpose of this research is to investigate and characterize the time-dependent
behavior of new concrete compositions made by replacing cement with secondary aggregates
— small clay particles — and then comparing them with control specimens made from
standard concrete. Cement is one of the main constituents of standard concrete, but the
carbon dioxide released into the atmosphere during the cement production process
contributes to the global warming and the development of holes in the ozone layer. The use of
clay particles in concrete production can make the construction industry more
environmentally friendly. This paper presents experimental test results of the compression
creep of the proposed concretes. Several concrete compositions with unconventional
additives were designed and prepared. The tests were performed on both normal strength and
high strength concretes. Specimens were tested in two extreme environments: in one case
there was 100% humidity provided by protecting the specimens from desiccation, and in the
other case specimens were air-dried and protected from any moisture. Concrete specimens
were subject to load in a constant room temperature and with a constant level of moisture.
The investigated properties include compression strength, modulus of elasticity and creep.
The creep test results showed that after approximately 90 days of loading, the response
seemed to be smaller for high strength concretes than for normal strength concrete.

Keywords: creep, montmorillonite nano particles, compression strength, modulus of

elasticity, creep coefficient
INTRODUCTION

The deformation characteristics of concrete are important in the design of sustainable

structures. Concrete is an important structural material used in every country of the world.
Moreover, the complexity of structures and their size have continued to increase, and this has
resulted in a greater importance of their deformation characteristics and in more serious
consequences of their behavior [4]. One type of strain that plays a major role in successful
and continuous use of structures is creep – deformations that appear due to long-term loading
of the structural element [3].

Formulation of creep and relaxation models has been ongoing from more than hundred years.
In the case of concrete, elastic behaviour of concrete was taken for granted for a long time.
However, in 1907 Hatt wrote an article on a test performed on reinforced concrete beams
subjected to constant load. Hatt discovered that the deflection increased significantly with
time [7].

Creep of concrete originates in the hardened cement paste that consists of a solid cement gel
containing numerous capillary pores. The cement gel is made up of colloidal sheets of
calcium silicate hydrates separated by spaces containing absorbed water. Creep is thought to
be caused by several different and complex mechanisms not yet fully understood. Neville et
al. identified the mechanisms for creep. Recent research relates the creep response to the
packaging density distributions of calcium-silicate-hydrates. At high stress levels, additional
deformation occurs due to the breakdown of the bond between the cement paste and
aggregate particles [4].

Therefore, designers and engineers need to know the creep properties of concrete and must be
able to take them into account in the structure analysis. After all, the end product of an
engineer's endeavours is a structure whose strength is adequate, but not wastefully excessive,
whose durability is commensurate with the conditions of exposure, and whose serviceability
ensures fitness for the purpose. Consideration of creep is a part of a rational approach to
satisfying these criteria. Deformation characteristics of materials are an essential feature of
their properties, and a vital element in the knowledge of their behaviour. After all, it is the
subject that matters: creep is important if its deformation increases with time under a constant
stress [4].

Nowadays nano-particles of clay minerals are used in production of polymeric

nanocomposite in order to improve mechanical characteristics. Polymeric nanocomposites
had been developed by Japan scientists in 1970 – 80th. In Latvia nanocomposites based on
styrene-acrylate copolymer and organically modified with montmorillonite nano particles
was prepared and investigated during recent 10 years [1].

Investigations on modifying concrete compositions by nano particles are carried out in

present time in different countries. It is proved that nanosized silicium dioxide particles allow
to achieve very dense microstructure and to improve performance characteristics of concrete
[1]. Information about montmorillonite nano particles use as concrete nano-filler not found in
literature. The aim of this study is to investigate influence of synthetized montmorillonite
clay mineral nano-particles (MNP) on mechanical strength and creep behavior of concrete.

Used material is synthesized montmorillonite clay mineral named as Hydrated sodium

calcium aluminum silicate, chemical formula (Na,Ca)(Al,Mg)6(Si4010)3(OH)6-nH20.
Montmorillonite mineral is a member of the smectite family. Montmorillonite crystal
structure is 2:1, meaning that it has 2 tetrahedral layers of silicium dioxide sandwiching a
central octahedral layer of aluminium oxide. Average density of montmorillonite clay mineral
is 2.35 g/cm3, specific surface 750 m2/g. The particles are plate-shaped, average length 20-
500 nm, Thickness of clay flakes about 1 nm, therefore clay may be classified as nano-
admixture [2].

METHODS

One of the goals of the experiment was to find out whether the new concrete composition can
be competitive and whether its physical and mechanical properties are equivalent to those of
ordinary concrete. The object of this experimental study was ordinary and high strength
concrete made with admixture of montmorillonite clay mineral nano particles (MNP) in
amounts of 1per cent of the total cement volume. Other raw materials used for this study
were natural coarse diabase aggregate, shingle, fine aggregate quartz sand and normal
portland cement CEM I 42.5 N. Table 1 shows concrete mix composition [2].

Table 1 Concrete mix compositions

MIX DESIGNATION HSC HSC MNP REFERENCE MNP

Portlandcement CEM I 42.5 N 800 800 350 350
Diabaze 0/5 mm 640 320
Shingle 5/20 500 500
Shingle 2/12 500 500
Sand 0/2.5 640 320 750 750
Silicafume 120 120 80 80
MNP 8 3,5
Water 200 200 190 190
Superplasticizer 15 15 7 7
Water/ Cement ratio 0.25 0.25 0,54 0,54

Standard sample cubes 100x100x100 mm and prisms 40x40x160 mm were produced in order
to investigate the mechanical characteristics of the material. Concrete mixtures were cast into
oiled steel moulds and compacted at the vibrating table. After two days the moulds were
removed. Standard hardening conditions (temperature +20 ± 1ºC, RH > 95%) were provided.
After the hardening period, the samples were measured and tested in standard conditions.
Their compression strength was determined in conformity with LVS EN 12390-3:2002.

At the beginning of the creep test, the specimens were 51; 57 and 63 days old. The tests were
conducted in two extreme conditions. In one case no moisture exchange with the environment
was permitted, which was ensured by protecting the specimens against desiccation, and in the
other case drying was permitted under conventional conditions, by protecting the specimens
against moisture [5]. In this paper shall be called these batches Reference (dry), Reference
(moist), MNP (dry), MNP (moist), HSC MNP (dry) and HSC MNP (moist). In order to
prevent humidity exchange between the specimen and the environment, the surface of the
specimens was coated with two protective silicone layers. Before this sealing, four aluminium
plates were centrally and symmetrically glued onto two sides of the test prism in order to
provide a basis for the strain gauges. The distance between two plates was 50 mm. Two +/-
0.01 mm precision strain gauges were symmetrically connected to each specimen, and then
the specimens were put into a creep lever test stand and loaded. Figure 1 shows the creep
lever test stand. Specimens were kept in a dry atmosphere of controlled relative humidity in
standard conditions: temperature 23 ± 1ºC and relative humidity 25 ± 3%.

Consider a point in a concrete specimen subjected to a constant, sustained compressive stress

σc0 applied at time τ0 and equal to 30 per cent of the characteristic compressive strength of
concrete for high strength concrete mixes specimens i.e. σc0= 0.3 fc and 40 per cent for
ordinary concrete mixes specimens, i.e. σc0= 0.4 fc [5, 6]. Load was applied gradually in
4 steps and as quickly as possible.

They were kept under constant load for 90 days and for recoverable creep they were kept
without load for 40 days.

Figure 1 Specimens in the creep lever test stand

Equation 1 shows the instantaneous strain that occurs immediately upon application of the
stress:

 e(t )   c / Ec (1)

where Ec is the elastic modulus at time τ0

 e(t ) is the instantaneous strain
 c is the compressive stress

Equation 2 shows the creep strain  cc (, t o ) in time t () subjected to a constant sustained
compressive stress σc applied at age t0:
  cc (, to )  (, to )   c / Ec (2)

where  cc (, t o ) is the creep strain

 (, to ) is the creep coefficient

Equation 3 shows the capacity of concrete to creep is usually measured in terms of the creep
coefficient  (, to ) . In a concrete specimen subjected to a constant sustained compressive
stress  c , first applied at age t, the creep coefficient at time t is the ratio of the creep strain to
the instantaneous strain [3]:

(, to )  cc (, to ) / e(t ) (3)

RESULTS

The tests to determine compression strength, modulus of elasticity and creep, creep
coefficient were done on concrete samples in which montmorillonite nano particles (MNP)
were used as admixture. Experimental work made it possible to compare the strength of
reference concrete samples and samples containing MNP.

Cubes’ strength tests were carried out after 7; 37; 42 and 93 days of hardening in standard
conditions. The various compression strengths of concrete specimens in different ages
containing MNP as an aggregate were then compared to reference concrete specimens. Figure
2 shows that HSC MNP was 5% lower strength in the first 7 days, but on the 37th day the
strength increased and was by about 4.8% larger than HSC, and on the 93rd day the strength
of concrete with MNP was larger by about 3.5%.

Figure 2 Concrete compression strength at 7; 37; 42 and 93 days, MPa

Ordinary concrete containing a MNP showed 31.4% lower strength in the first 7 days than
reference concrete strength and on the 42nd day the strength was lower by about 32.4%.
High strength concrete mix containing montmorillonite nano particles perform good strength
development during long-term hardening period. HSC MNP specimens showed a 45.8%
increase of compression strength, while the HSC showed a 33.8% increase of compression
strength on the same period. Ordinary concrete specimens with a MNP showed a 48.5%
increase of compression strength, but the reference specimens showed a 50.8% increase of
compression strength.

Figure 3 shows that the modulus of elasticity was determined by measuring the deformations
on the sides of the specimens according to Hooke's law. For HSC at the age of 51 days the
difference between specimens hardened in moist and dry conditions is approximately 1.9%
but at the age of 63 days the difference is 16%. For HSC MNP this difference is
approximately 17.4% and 11% respectively. The comparison of the modulus of elasticity of
51 days old HSC and HSC MNP specimens shows that the modulus of elasticity for
specimens with montmorillonite nano particles is larger. For specimens hardened in moist
conditions this difference is 34.5%, while for samples hardened in dry conditions it is 9%.
However, the comparison of the modulus of elasticity of 63 days old HSC specimens and
specimens containing MNP shows contrary results – the modulus of elasticity for HSC
specimens is larger. For specimens hardened in moist conditions this difference is 43.5%,
while for samples hardened in dry conditions it is 6.2%.

Figure 3 Modulus of elastisy of different concrete

Figure 3 shows that for reference concrete and for concrete specimens with MNP this
difference between specimens hardened in moist and dry conditions are approximately 17%
and 16% respectively. The comparison of the modulus of elasticity of reference concrete
specimens and specimens with MNP shows that for specimens hardened in moist conditions
this difference is 3.3%, while for specimens hardened in dry conditions it is 24%.
Figure 4 the stress-strain relation shows that the same tendency. The stresses are almost
proportional to the strain, and therefore the stresses do not reach the point of microcracking.

In a loaded specimen that is in hygral equilibrium with the ambient medium (i.e. no drying),
the time-dependent deformation caused by stress is known as basic creep [4]. Creep increases
with time at a decreasing rate. In the period immediately after initial loading, creep develops
rapidly, but with time the rate of increase slows considerably [3].

Figure 5 shows elastic strain plus linear basic creep and shrinkage as dependence of time.
Under constant mechanical loading, the strain of HSC at the ages of 51 and 63 days increases
significantly with the loading duration, the increase reaching 2.6 to 3.3 times the value of the
instantaneous strain. At both ages, the strain increase of concrete specimens containing MNP
reaches 2.6 to 4.8 times the value of the instantaneous strain.

Figure 4 Relation between stress and strain

The smallest deformation was exhibited by HSC in moist conditions. The average difference
between HSC specimens hardened for 51 days in moist and in dry conditions is
approximately 23% and the smallest creep is for specimens in dry conditions, but for HSC
specimens at the age of 63 days hardened in moist and in dry conditions the amount of
deformations is contrary – the creep is larger in dry-hardened specimens, and the average
difference is approximately 30%. For 51 days old HSC MNP specimens this difference is
approximately 46%, and for 63 days old specimens it is 28%. At both ages the larger
deformation was exhibited by dry-hardened specimens. If we compare the average difference
between the HSC specimens at 51 days and the HSC MNP ones of the same age, we can see
that for specimens hardened in moist conditions this difference is 23%, and for specimens
hardened in dry conditions it is 85%. In moist conditions the larger deformation is exhibited
by HSC specimens, but in dry conditions it is contrary – the larger deformation is exhibited
by HSC MNP specimens. In comparison with the 63 days old specimens, the difference is
38% and 24% respectively. In dry condition smaller deformation is shown by HSC specimens
for both ages and in moist condition smaller deformation is by HSC containing MNP for both
ages.

Figure 5 shows that under constant mechanical loading, the strain of reference concrete
increases significantly, the increase reaching 3.15 to 3.61 times the value of the instantaneous
strain, and for specimens containing MNP it reaches 2.88 to 4.32 times. The smallest creep is
exhibited by reference concrete specimens in dry conditions. The average difference between
basic creep of reference concrete specimens hardened in moist and in dry conditions is
approximately 21%. For specimens containing MNP this difference is approximately 14.5%.
By comparing the average difference between the reference concrete specimens and the MNP,
it can be seen that for specimens hardened in moist conditions this difference is 12.8%, and
for specimens hardened in dry conditions it is 22%.

Figure 5 shows recoverable and irrecoverable creep. Largest part of recoverable creep strain
is instantaneous. At both ages for HSC the larger difference of irrecoverable creep strain was
exhibited by moist-hardened specimens but for HSC MNP specimens it is contrary – the
larger difference is exhibited by dry-hardened specimens.

The creep coefficient increases with time at an ever-decreasing rate. The final creep
coefficient is a useful measure of the creeping capacity of concrete.

Figure 5 Elastic strain and long-term deformations of different kind concrete samples

Figure 6 shows the comparison of the creep coefficients of HSC and HSC MNP
specimens at the age of 51 days. The creep coefficient for specimens in dry conditions
with clay particles is larger but in moist conditions the creep coefficients are similar but at
the age of 63 days the creep coefficients of dry-hardened specimens are similar, while in
specimens cured in moist conditions the creep coefficient of concrete specimens
containing MNP is smaller. The average difference between HSC specimens at the age of
51 days hardened in moist and in dry conditions is approximately 19%, but for HSC
specimens at the age of 63 days hardened in moist and in dry conditions the coefficient is
larger for dry specimens. The difference is approximately 5%. At both ages the larger
coefficient is exhibited by moist-hardened specimens. For 51 days old MNP specimens
this difference is approximately 50%, and for specimens at the age of 63 days it is 48%.
At both ages the larger coefficient is exhibited by dry-cured specimens. If compare the
average difference between 51 days old HSC specimens and the ones containing MNP
than for samples hardened in moist conditions this difference is 10%, and for samples
hardened in dry conditions it is 104%. In comparison with the 63 days old specimens, the
difference is 29% and 11% respectively. Interesting that in moist conditions the larger
coefficient is exhibited by HSC specimens, but in dry conditions the larger coefficient is
shown by specimens containing MNP, but in moist conditions the smallest coefficient is
exhibited by specimens containing MNP, but in dry conditions the smallest coefficient is
shown by HSC specimens.

Figure 6 Creep coefficients of different kind concrete samples

The comparison of the creep coefficients of reference concrete specimens and MNP
specimens shows that the creep coefficient of specimens containing clay particles and
hardened in dry conditions is larger but in the moist conditions the creep coefficient is larger
for reference concrete. The average difference between reference concrete specimens in moist
and in dry conditions is approximately 10%, but for MNP specimens this difference is
approximately 27%. If we compare the average difference between reference concrete
specimens and the ones containing MNP we can see that for specimens hardened in moist
conditions this difference is 15.4%, and for specimens hardened in dry conditions it is 6.5%.
 CONCLUSIONS

This experimental study proves that montmorillonite nano particles in small dosage (8 kg
in m3) don't have negative influence on mechanical and deformation characteristics of
concrete. Some positive effects are established. Long-term deformation testing was
carried out, and the modulus of elasticity and the compression strength of ordinary
concrete and of concrete containing montmorillonite nano particles were determined.

High strength concrete mix containing montmorillonite nano particles perform long-term
hardening effect. Compression strength of 93 days old high strength concrete specimens
containing MNP was larger than that of HSC specimens. Ordinary reference concrete
specimens and specimens containing MNP showed a similar increase of compression strength
at both ages.

The modulus of elasticity in dry condition at all ages was larger for reference specimens,
but in moist condition it was larger for concrete specimens containing MNP.

The smallest basic creep in dry conditions is for reference concrete specimens and in
moist condition for concrete specimens containing MNP. Largest part of recoverable creep
strain is instantaneous.

The final creep coefficient is a useful measure of the creep capacity of concrete. On the
90th day of testing, the value of the basic creep coefficient reaches 1.5 to 2.8 for HSC
specimens and 1.7 to 4.1 for concrete specimens containing MNP. And for ordinary
concrete the value of the basic creep coefficient reaches 3.1 to 3.6 and 2.8 to 4.3 for
concrete specimens containing MNP. The results of this experiment can be used to predict
creep deformations.

In the future, the physical and mechanical properties of new high-strength concrete
containing montmorillonite nano particles as an alternative admixture should be
investigated in a more detailed way. Possibilities to increase efficiency of
montmorillonite nano particles must be regarded. Particle additional chemical treatment
or thermal activation may be used in future research.

Obtained results indicate on quite high dispersion of experimental data. In order to

decrease the dispersion of results, the number of specimens and tests should be increased.

ACKNOWLEDGEMENT

This work has been supported by the European Social Fund within the scope of the project
―Support for the Implementation of Doctoral Studies at Riga Technical University‖.

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