Dr.ing. thesis by Bård M.

Pedersen:

“Alkali-reactive and inert fillers in concrete. Rheology of fresh

mixtures and expansive reactions”

Norwegian University of Science and Technology,

Department of Structural Engineering.

Abstract
Due to the rather limited obtainable resources of natural aggregates suitable for
concrete purposes, the technology of crushed aggregates becomes more important.
The production of crushed aggregates generates large amounts of fines or fillers,
presently to some extent considered to be leftovers. From an environmental point of
view, as well as from an economic point of view, it is important to be able to utilize
these fines. Because of the large surface area of the filler fraction of the aggregate, the
addition of filler may modify the rheological properties of fresh concrete to a great
extent. Recently, the need for good fillers has increased due to the development of
self-compacting concrete. To attain the much higher flowability of self-compacting
concrete compared to ordinary vibrated concrete, the volume of the fluent phase, i.e.
the matrix phase, has to be increased. At the same time, the self-compacting concrete
has to be stable. The addition of filler may then be beneficial from a technical point of
view. In addition, the use of fillers may be more cost efficient than other possible
solutions.

There are examples in the literature that fillers may modify the properties of the
hardened state as well as the properties of the fresh state of concrete. Fillers have been
reported to accelerate the cement hydration in some cases. Examples of increased
compressive strength also exist. This is believed to be due to a general filler effect, i.e.
that the cement hydration products may grow faster and become more evenly
distributed in the presence of small mineral particles. In addition to the general filler
effect, there might be chemical effects, in some cases pozzolanic reactions.

The present study has focused on fillers classified as alkali-reactive. The alkali-silica
reaction in concrete is known to result in cracking and overall expansion of structural
elements. There are some examples in the literature indicating that the finest particles
of alkali-reactive aggregates should not be considered dangerous in concrete. Some
researchers have reported that filler particles below a critical limit, which has been
reported to be in the order of 50 µm for some rocks, may give pozzolanic reactions,
and consequently be beneficial. However, there have been reported cases where
particles smaller than 20-30 µm gave very fast and deleterious reactions. In the present
study, alkali-reactive fillers from two Norwegian cataclastic rocks have been
investigated. The study has included fillers of Icelandic glassy rhyolite and crushed
bottle glass. Non-reactive reference fillers were included in the study, as well as silica
fume and fly ash known to mitigate alkali-silica reactions.

The direct pozzolanic reactivity of the fillers has been quantified by mixing calcium
hydroxide, filler and artificial pore water. The loss of calcium hydroxide over time
measurd by TGA is then a direct measure of the pozzolanic reactivity. When testing
the 0-20 µm fractions of the different fillers at 20ºC, the materials could be divided
into two distinct classes with respect to pozzolanity:

• The pozzolanic reactivity of fly ash, glass and rhyolite filler was distinct
• The pozzolanic reactivity of mylonite, cataclasite and quartz fillers was
insignificant at the age of 28 days

All the materials being highly pozzolanic have a distinct amorphous silica phase,
while the silica phase of the non-pozzolanic materials is well crystalline quartz. The
known deformation and sub-grain development due to cataclasis of the tested reactive
Norwegian rocks does not seem to increase the pozzolanic reactivity much.

The mylonite filler has also been tested at curing temperatures of 38ºC and 80ºC. The
pozzolanic reactivity was very low also at 38ºC. However, at a temperature of 80ºC,
corresponding to the temperature used by the accelerated mortar bar test, the
pozzolanic reactivity was significant. Non-reactive granite/gneiss filler of glacioflucial
origin was also pozzolanic at 80ºC. It may then be suggested that all fillers of rocks
containing silica will be more or less pozzolanic at such high temperatures as 80ºC.

Based on testing by the concrete prism method, the fillers could be divided into two
distinct classed with respect to their effect on alkali-silica reactions in concrete:

• Fly ash, silica fume, glass filler and rhyolite filler significantly reduced the
expansions compared to the reference concrete
• Mylonite and cataclasite filler had no effect or gave increased expansions
compared to the reference concrete

These results are based on experiments by the concrete prism test, which is believed to
provide a realistic picture of the real behaviour in field conditions. Micro structural
analyses, using optical microscopy and electron probe micro analyser, have given
additional information regarding the performance of glass filler, mylonite filler and
rhyolite filler compared to the reference concrete, and confirmed the expansion results
of the concrete prism test.

The effect of the tested fillers with respect to alkali-silica reactions matched their
pozzolanic reactivity. Fillers being highly pozzolanic reduced the expansions due to
ASR, while non-pozzolanic alkali-reactive fillers gave in most cases increased
expansion compared to the reference mix. Consequently, such alkali-reactive fillers
should be treated as potentially deleterious in concrete.

The accelerated mortar bar test has been widely used around the world to test the
effect of different additives, such as silica fume, fly ash and slag. Other additional
materials, such as crushed bottle glass, have also been tested using this method. Some

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studies have indicated a rather strong correlation between the results obtained by
concrete prism testing and results obtained by accelerated mortar bar testing. In the
present study, extensive testing of fillers by the accelerated mortar bar test was carried
out to give a preliminary screening of the materials. Testing of rhyolite filler, glass
filler, fly ash and silica fume reduced the expansions significantly compared to the
reference mortar when tested by the accelerated mortar bar test. This is in accordance
with the results obtained for the same fillers by the concrete prism test. However, the
accelerated mortar bar test also predicted the Norwegian reactive rock fillers to inhibit
expansions due to alkali-silica reactions. This contradicts the predicted effect of these
fillers by the concrete prism test. Testing of non-reactive limestone filler gave no
effect at all on mortar bar expansion. This indicates that the effect of the Norwegian
reactive rock fillers by this method is due to chemical, and not physical effects. Due to
the high temperature used by the accelerated mortar bar test (80ºC), the quartz in these
rock fillers are believed to react pozzolanic. Methods such as the accelerated mortar
bar test, or other methods using very high temperatures, should consequently not be
used to evaluate the effect of rock fillers containing silica, unless their pozzolanic
reactivity are evident also at lower temperatures.

The pozzolanic materials (fly ash, silica fume, rhyolite and glass filler) gave a
significant increase in compressive strength. This is believed to be due to their
pozzolanic reactivity. No significant effect on the compressive strength of any of the
Norwegian rock fillers (mylonite, cataclasite and granite/gneiss filler) was noticed at
normal filler addition levels.

The present study has given valuable information concerning the practical
implications of using alkali-reactive fillers. The similarity between the alkali-silica
reaction and the pozzolanic reaction has been highlighted. However, some of the more
fundamental issues concerning the paradox of the alkali-silica reaction and the
pozzolanic reaction are still far from being fully understood, and it is clear that more
basic research is needed in this area.

Testing of the effects of fillers on the rheological properties of fresh concrete was
done by matrix testing within the present study. The matrix refers to the fluent phase
of the particle-matrix model. It consists of the cement paste and all powders of particle
size < 0.125 mm, including the aggregate filler. Some of the limitations of the particle-
matrix model with respect to self-compacting concrete have been treated in the present
study. The characterisation of the matrix phase by simple flow viscometers are
believed to be insensitive to the small, but significant, changes in yield stress. A more
fundamental characterisation of the matrix phase has been introduced. By using the
Physica rheometer with parallel plate configuration, the fundamental measures yield
stress and plastic viscosity could be obtained.

The effect of fillers on the flow resistance ratio of the matrix has been tested. As
expected, addition of filler increased the flow resistance ratio. The effect of the
different fillers varied much, to a large extent due to the variations in particle size
distribution. The granite/gneiss filler, which is coarse compared to the crushed rock
fillers, gave the lowest flow resistance ratio. Fly ash, which has a particle size
distribution similar to cement, gave the highest flow resistance ratio. Replacement of

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cement by filler reduced the flow resistance ratio for most of the fillers. The exception
was fly ash and glass filler, which gave the opposite effect. In addition to the particle
size grading of the fillers, the mineralogy seems to haves some influence. In this
respect, limestone filler gave rather low flow resistance ratios in relation to its fine
particle size distribution.

A laboratory program using the Physica rheometer to give a more fundamental

characterisation of the effects of filler on the matrix has been carried out. The plastic
viscosity obtained from testing by the Physica rheometer is more or less an equivalent
measure to the empirical flow resistance ratio obtained by the FlowCyl testing.
Consequently, the effect of the fillers with respect to plastic viscosity was basically
equal to their effect on flow resistance ratio. The replacement of cement by filler has
been shown to alter the rheological properties significantly. Generally, fillers gave
lower yield stress and plastic viscosity than equal volumes of cement. An increase in
plastic viscosity was generally followed by an increase in yield stress. However, it has
been shown that the ratio between yield stress and plastic viscosity is highly
dependent on the type and dosage of plasticizer. The new co-polymers generally
reduced the yield stress to a much higher extent than lignosulphonate or naphthalene.
Further, the co-polymer seems to level out the large differences due to different fillers,
which may be apparent when using other types of plasticizers. Also the cement type
has been shown to influence the ratio between yield stress and plastic viscosity
largely.

A study of the relationship between the rheological properties of the matrix phase and
self-compacting concrete has indicated that the yield stress of the matrix phase has a
crucial influence on the empirical slump-flow measure. No straightforward correlation
between the rheological properties of self-compacting concrete and the corresponding
matrix phase was found. Studies on rheological properties of the matrix phase should
be considered useful to gain fundamental knowledge regarding the effects of different
constituents. Matrix testing may to some extent be useful to predict the effects in self-
compacting concrete, but the limitations should be kept in mind when using matrix
results to predict the behaviour of a given constituent in concrete. The study has
confirmed the basic principles of the particle-matrix model for self-compacting
concrete. However, further work is needed to go deeper into the very complex
relationship between the concrete rheology and the matrix rheology.