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Early Age Properties of SCC
Early Age Properties of SCC
self-compacting concrete
– Effects of fine aggregate and limestone filler
OSKAR ESPING
OSKAR ESPING
Chalmers Reproservice
Göteborg, Sweden 2007
ABSTRACT
Self-compacting concrete (SCC) is a sensitive mix, strongly dependent on the composition
and the characteristics of its constituents. It has to possess the incompatible properties of
high flowability together with high segregation resistance, a balance made possible by the
dispersing effect of water-reducing admixture combined with cohesiveness produced by a
high concentration of fine particles. These fines and their effects on the early age
properties of the SCC have been in focus in this present dissertation.
The effect of the specific surface area of gravel and limestone filler on the rheology of
SCC was evaluated. Performed experiments clearly demonstrated that traditional methods
for geometric characterization of the fines (size distribution, water absorption, fineness
modulus, etc.) are not sufficient to ensure consistent quality of SCC. By measuring the
specific surface area with a simplified gas adsorption method, BET(H2O), it was found that
the specific surface area of a normal gravel, accepted by traditional methods for production
of SCC, can vary up to 7000 m2/kg. A model is proposed, based on an assumption that 30
full molecular layers of water covering the particle surface are required to provide
lubrication sufficient to create flowability, where a change in specific area is translated to a
change in water demand for the concrete mix. It is suggested that an increase in
BET(H2O)-area of 1000 m2/kg corresponds to an increase in water demand by
approximately 0.85% by mass of the filler or gravel content for constant flowability.
Furthermore, the influence of mix design and fines BET(H2O)-area on the SCC’s early-age
deformation was demonstrated. The autogenous (sealed) deformation was measured with a
specially developed concrete dilatometer, together with capillary pore pressure and
temperature. It is suggested that that autogenous shrinkage and rate of evaporation are the
main factors promoting the risk of plastic shrinkage cracking. An increased particle surface
decreased the rate and magnitude of evaporation, and consequently reduced the plastic
cracking tendency, despite an increase in autogenous shrinkage.
The work presented in this doctoral thesis is based on the following papers, referred to in
the text by their Roman numbers:
I. Slump flow values vs. Bingham parameters for high flowable mortars and
concretes
Esping O., Accepted for publication in 5th International RILEM Symposium on
Self-Compacting Concrete, 3-5 September 2007, Ghent, Belgium, 2007.
II. Methods for characterisation of fillers and fines for self-compacting concrete
Esping O., 3rd International RILEM Symposium on Self-Compacting Concrete,
PRO 33, 17–20 August, pp 208-219, Reykjavik, Iceland, 2003.
III. SCC flowability: Effect of changes in particle surface area, and how to
compensate for this
Esping O., Accepted for publication in 5th International RILEM Symposium on
Self-Compacting Concrete, 3-5 September, Ghent, Belgium, 2007.
ABSTRACT III
APPENDED PAPERS IV
CONTENTS V
NOTATIONS VIII
1 INTRODUCTION 1
1.1 Background 1
1.2 Objective and limitations 2
1.3 Disposition of the thesis 3
1.4 Original features 3
2 RHEOLOGY 5
2.1 Introduction 5
2.2 Particle suspensions 7
2.3 Measuring techniques 22
2.4 Concluding remarks 27
3 EARLY-AGE DEFORMATION 29
3.1 Introduction 29
3.2 Plastic shrinkage cracking 31
3.3 Mechanisms of early-age deformation 32
3.4 Measuring techniques and methods 42
3.5 Concluding remarks 47
4 EXPERIMENTAL WORK 49
4.1 Introduction 49
4.2 Materials and mix design 50
4.3 Particle quantifications 53
4.4 Mortar and concrete quantifications 62
4.5 Concluding remarks 72
6 REFERENCES 79
APPENDIX A: BET(H2O) 91
The work presented in this doctoral thesis is one of the two outcomes of the project
“Industrial building with in-situ cast concrete – New concepts”, which was made possible
by a donation from Thomas Concrete Group / AB Färdig Betong to Chalmers University of
Technology. The work has been conducted at the Department of Civil and Environmental
Engineering (Chalmers University of Technology) and at the research centre of Thomas
Concrete Group in Göteborg, during the period 2001-2007. During the first years this
thesis was carried out under the supervision of Professor Lars-Olof Nilsson now at Lund
University of Technology, and during the remaining years under Professor Tang Luping
at Chalmers University of Technology. Professor Per-Erik Petersson at the Swedish
National Testing and Research Institute has acted as assisting supervisor. I am most
grateful for their support and assistance.
Grateful thanks are also addressed to:
☺ Annika Wirje, Färdig Betong AB
☺ Jan-Erik Lindqvist, Swedish National Testing and Research Institute
☺ Martin Hansson, Sika
☺ Mats Karlsson, Thomas Concrete Group AB
☺ Mette Geiker, Technical University of Denmark
☺ Olafur Wallevik, The Icelandic Building Research Institute
☺ Peter Billberg, Swedish Cement and Concrete Research Institute
☺ Sten Rodenstam, Nordkalk AB
Special thanks are due to Thomas Concrete Group and AB Färdig Betong for their
generous donation, support and confidence in me.
I would like to extend my special thanks to Ingemar Löfgren and Professor Tomas Kutti
at Thomas Concrete Group AB for their involvement in this work, and for their
indispensable help, guidance, encouragement and always valuable advice.
Finally, I would like to thank my future wife, Lotta, and children Albin and Elin, for
supporting and having patience with me during my doctoral studies.
It is my hope that this paper will be reviewed critically. Any viewpoints, comments and
suggestions about the text should be directed to me.
By the nature of an experimental investigation, each question is often answered with many
new questions. And with knowledge arises a question whether the experimental course of
action could be made in a more proper way. It ought to be noted that the purpose of a PhD
study is educational, and that the work presented in this doctoral thesis is mainly intended
as a personal learning process, not to produce unique or useful results. Yet it has to be
performed with a scientific approach and to fulfil certain requirements of quality, which I
hope to have achieved for the benefit of future research.
Abbreviation Description
A aggregate
ACC accelerator
C cement
BET Brunauer, Emmet, and Teller
CDD concrete digital dilatometer
CH calcium hydroxide
C-S-H calcium silicate hydrate
COV coefficient of variance
F filler
H2O (see W)
LOI loss of ignition
N2 nitrogen
P powder
RE retarder
SCC self-compacting concrete
SEM scanning electronic microscopy
SF silica fume
Size size distribution
SP superplasticizer
SRA shrinkage reducing admixture
W water
1 INTRODUCTION
1.1 Background
Cement-based materials are the most abundant of all man-made materials and are among
the most important construction materials, and it is most likely that they will continue to
have the same importance in the future. However, these construction and engineering
materials must meet new and higher demands. When facing issues of productivity,
economy, quality and environment, they have to compete with other construction materials
such as plastic, steel and wood. One direction in this evolution is towards self-compacting
concrete (SCC), a modified product that, without additional compaction energy, flows and
consolidates under the influence of its own weight.
The use of SCC offers a more industrialised production. Not only will it reduce the
unhealthy tasks for workers, it can also reduces the technical costs of in situ cast concrete
constructions, due to improved casting cycle, quality, durability, surface finish and
reliability of concrete structures and eliminating some of the potential for human error.
However, SCC is a sensitive mix, strongly dependent on the composition and the
characteristics of its constituents. It has to possess the incompatible properties of high
flowability together with high segregation resistance. This balance is made possible by the
dispersing effect of high-range water-reducing admixture (superplasticizer) combined with
cohesiveness produced by a high concentration of fine particles in additional filler material
[1]. The main mechanisms controlling this fine balance are related to surface physics and
chemistry; hence, SCC is strongly dependent on the activity of the admixtures, as well as
on the large surface area generated by the high content of fines [2]. Fresh SCC, like all
cementitious materials, is a concentrated particle suspension with a wide range of particle
sizes (from 10-7 to 30 mm for concrete). The particles are affected by a complex balance of
interparticle forces (i.e. interlocking, frictional, flocculation, colloidal, van der Waals, and
electrostatic forces), generating a time dependence and viscoplastic non-Newtonian
behaviour. In addition, the concretes have irreversible time-dependent properties as a result
of the chemical reactions [3].
Since the ratio of surface area to volume increases exponentially with particle irregularity
and decreased size, this area has a predominant effect on fresh and hardened concrete [4]-
[7]. Particles with apparently similar grading can provide significantly different effects on
concrete properties. These differences can be related to the fineness, shape, surface texture,
porosity, etc. If the particles provide a large specific area, a large quantity of water will be
adsorbed on the particles’ surfaces and less water will be available to lubricate and disperse
the particles, which is needed to provide flowability [8]. This adsorption will also influence
the development of negative capillary pore pressure, causing the paste to contract [9].
These contracting capillary forces are inversely proportional to the meniscus radius, and
hence the capillary tension stresses increase with decreasing pore sizes and interparticle
spaces. As a consequence of the large surface area generated by the high concentration of
powder material, and the retarding effect of superplasticizer, the SCC may develop a large
autogenous shrinkage and thus a high plastic shrinkage cracking tendency [10].
As aggregates represent 60-80% of the total volume of concrete, it is obvious that their
influence on the fresh and hardened concrete is substantial. Properties of fine particles (<63
µm) and their influence are often neglected, because traditional standard methods for
characterizing aggregates are deficient. The content of fine particles, by volume or weight,
is often small but the number of particles and their total surface area are large. A content of
3 vol-% of particles finer than 63 µm (EN 933-1, or 75 µm according to ASTM C33) is
considered harmful, but these particles and their surface properties may have a
considerable influence on the quality of the concrete, in either fresh or hardened state [8].
Powder material (filler, cement, etc.) is traditionally characterized by its size distribution
and specific surface area by Blaine. Due to the methodology, where the surface area is
determined by air permeability, based on packed spherical particles, information about the
shape, texture and surface porosity is neglected [5][11]. An irregular and porous particle
can provide a considerably larger surface area, accessible to water, than a spherical one
(see Figure 1). Under real conditions, a particle external surface can be as much as 1000
times greater that that of a sphere with equal volume [12]. Other, possibly more correct,
methods for geometric characterization, such as the BET with nitrogen gas or image
analysis, are more seldom used due to their complexity and high cost.
Hence, to be able to offer a high-quality product, it is imperative to have understanding and
knowledge of how the constituents affect the concrete’s fresh and hardened properties, and
how to characterize the concrete and its constituents’ properties.
Specific surface area - Particel geometry
70000
60000
50000 sphere
Area, S [m 2/m 3 ]
Irregular (5x)
40000
Irregular (10x)
30000
20000
10000
0
0.001 0.01 0.1 1
Size, D [mm] (log)
Figure 1. The enlarging effect of size (logarithmic) and shape on specific surface area,
illustrated with a spherical particle and an irregular one (with same section area but 5 and
10 times larger perimeter).
admixtures (especially the superplasticizer) predominate for the properties of fresh SCC,
and their effects have not been examined in this work. Nether have the thermal effects on
early-age deformation been considered. Methods for evaluation of specific surface area,
and correlation of measurement results from these methods with flow behaviour of mortars
and concretes, comprised a main topic. The concrete is structurally divided into two stages:
early age and long term, where early age is limited to 24 hours from mixing.
Rheologically, the concrete is also divided into two stages: fresh and hardened, where the
concrete (or mortar) is considered to be fresh as long as the matrix of suspended particles
is, or can be turned into, a liquid.
2 RHEOLOGY
2.1 Introduction
Rheology is defined as the science of deformation and flow of matter, and describes the
interrelation between force, deformation, and time [13]-[15]. It is normally applied to more
or less fluid materials, or materials that exhibit a time-dependent response to stress. An
important issue of rheology is the definition and classification of materials. One way to
characterize a material is by its relaxation time, i.e. the time required to reduce a stress in
the material by flow (see Table 1). Glass, for instance, is usually defined as a solid
material, but over a longer times perspective it flows like a liquid, although extremely
slowly.
Table 1. Classification of materials state in terms of their relaxation time (at 20ºC).
Gases Liquids Solids
Relaxation time [seconds] <10-6 10-6 – 100 >100
Another way of defining materials rheologically is by their flow characteristics, with a
classification into viscous, elastic and viscoelastic. Gases and many liquids are defined as
viscous. An ideal fluid is unable to store any deformation energy; when subject to stress, it
flows and the deformation energy is dissipated as heat (resulting in a rise of temperature).
Solids, on the other hand, can be described as elastic materials. Ideal elastic material stores
all imposed deformation energy, and will consequently recover totally upon a stress
release. But a large number of materials are viscoelastic (both viscous and elastic), i.e. they
store some of the deformation energy in their structure while some is lost by flow. The
simplest model describing an ideal fluid’s flow characteristics, and the basis for classical
fluid mechanics, is Newtonian – with a linear relationship between shear stress (σ) and
shear rate ( γ& ), and with zero stress at zero rate. This behaviour is analogous to Hookean
behaviour for a solid (see Figure 2). However, many important fluids, such as polymers,
blood, foods, cosmetics, and concretes, show non-Newtonian plastic behaviour, in which
flow only initiates above some level of stress (i.e. yield stress), and once flow begins the
relationship between shear stress and shear rate is linear or non-linear. The non-linear
materials can be either shear-thinning or thickening, with or without yield stress. Materials
with thickening behaviour are not very common, especially among particle suspensions.
Shear stress, τ [Pa] Shear stress, σ [Pa]
Hookean Newtonian
•
Shear strain, ε [-] Shear rate, γ [1/s]
Figure 2. The Hookean behaviour in which stress is proportional to strain versus the
Newtonian behaviour in which stress is proportional to shear rate.
Some materials also have a time dependence due to a flocculated microstructure, where the
flow characteristics are influenced by the shear history of a material. These types of
materials are usually defined as thixotropic or anti-thixotropic. In general, equilibrium
measurements are desired, and the time dependence is minimized by pre-shearing the
material and destroying the sample’s structure in the test [13]-[15].
A suspension with a wide range of particle sizes comprises a complex balance of
interparticle forces (i.e. interlocking, frictional, flocculation, colloidal, van der Waals, and
electrostatic forces), which generates this time dependence and viscoplastic non-
Newtonian behaviour [4][13][16]-[18].
Other factors which affect the flow behaviour are the temperature, pressure, and pH. It is
generally desirable to maintain these at constant levels throughout an experimental
procedure, and this is normally done. The effect of pressure can be neglected, as it is very
small at atmospheric pressure [13].
The viscosity of different materials varies in a wide range (Table 2) as do the shear rates
they may be subjected to in different industrial processes (Table 3). To be able to
characterize a fluid, a proper model to mathematically describe the rheology must be
selected, together with a suitable instrument for measurements under realistic conditions.
In the literature, there are several theoretical models, instruments and measuring
techniques proposed to evaluate the flow behaviour of non-Newtonian fluids.
Table 2. Viscosity of some familiar Table 3. Typical range of shear rates of
materials at room temperature [13][19]. some familiar processes [13].
Viscosity Shear rate
Liquid Process
η [Pa·s] γ& [s-1]
Glass 1040 Lubricating 103 - 107
Asphalt 108 Rubbing 104 - 105
Molten polymers 103 Spraying and brushing 103 - 104
SCC 102 Mixing and stirring 10 - 103
Syrup 10 Chewing / swallowing 10 - 102
Mortar 1 Pumping / pipe flow 1 - 103
Olive oil 10-1 Extruding 1 - 102
Water 10-3 Levelling 10-2 - 10-1
Air 10-5 Sedimentation 10-6 - 10-3
The rheological properties of cementitious materials (cement paste, mortar and concrete)
are mainly influenced by the following factors [5][20]-[24]:
a) Water content.
b) Amount of filler and aggregate, its particle shape, surface texture, porosity, size, and
size distribution, and consequently the particle packing and specific surface area.
c) Type and amount of cement and cement replacements
d) Amount of entrained air, and bubbles’ size.
e) Presence and efficiency of admixtures affecting the properties of adsorbed water
layer and particle dispersion.
f) Temperature.
g) Degree of hydration.
h) Time elapsed after mixing.
i) Mixing procedure.
Here, the water content and specific surface area are the two single most important factors
influencing the rheological properties of cementitious materials [5][22].
The objective of this chapter is to present, through a literature review, an introduction to
the rheology of particle suspensions and the factors affecting it. Flow behaviours,
rheological characteristics, models, and methods for measuring the rheology of fresh
cementitious materials are in focus.
where φ is the volume fraction of solids, and A and B are a constants (typically in the range
of A is 2–4). Another way to express the yield stress is to consider also interparticle forces
that are responsible for flocculation. The effect of w/c on yield stress (σy) can then be
calculated as:
ϕB
σ y = A⋅ 2
⋅ Φ max
'
[Pa] (Eq. 4)
r
where r is the particle radius, and Φ’max is the maximum interparticle force (maximum
slope of the pair potential) [25][26].
Coherence:
Flowability:
Liquid-need:
Attraction:
Repulsion:
Figure 3. Illustration of how particles of a certain size group under forces (x axis) are
acting in a suspension, in terms of coherence, flowability, need of liquid, and
attraction/repulsion (y axis). The magnitude is only relative within each property [18].
At macro-level there are interlocking and friction forces, and at micro-level there is a fine
balance between attractive and repulsive forces. The main attractive forces are collectively
called the van der Waals force (sometimes called London dispersion force), a short-range
electromagnetic and relatively weak force interacting between two bodies. The van der
Waals force arises from the polarization of molecules or particles into dipoles. This
includes forces that arise from fixed or angle-averaged dipoles (Keesom forces) and free or
rotation dipoles (Debye forces) as well as shifts in electron cloud distribution (London
forces) [4][27]. The main repulsive force is the force which the electrical double layer
gives rise to, and which acts between charged bodies with a potential difference.
The net result of these attractive and repulsive electric forces of suspended particles creates
an energy barrier as they approach each other [4]. The consequent potential energy, as a
+
concrete), where the fresh mix comprises a forces
Potential energy
complex balance of interparticle forces Interparticle
r0 r0’ distance, r
generating a suspension with viscoplastic non-
Newtonian behaviour. All these interacting
forces depend on the shape of the particles, Secondary
their size, concentration, and surface Attracting minimum
forces
properties, but also on the water content of the
-
In a matrix of the smallest particles, good coherence is accompanied by good fluidity (see
Figure 5). In a system with a wide range of particle sizes and all the forces working
together, the smallest particles with their good flowability now cause sedimentation of the
larger particles in the fluid matrix, and thus a bad coherence of the total mass. Hence, for
optimum coherence with strong flocculation, flowability is poor. This flowability can be
increased by adding more water as well as by increasing the amount of the smallest
particles, but at the price of decreased coherence. Thus, there is a compromise between
fluidity and coherence. Figure 5 illustrates how each group of particle sizes is affected by
another, in terms of coherence, flowability and need for water [4][18][24].
Hence, for a given mortar or concrete mix, the flowability can be adjusted on macro-level
by grading, shape and water content etc., and on the micro-level by the ratio between the
flocculation and colloidal forces. Stronger colloidal forces and weak coherence generate
better flowability, a smaller compaction energy need and a larger separation tendency [18].
Coherence:
Flowability:
Water-need:
Figure 5. When a suspension incorporates a mix of particle sizes, the forces are acting
together. The figure illustrates how this balance of different size groups forces (x-axis)
affects coherence, flowability and need for water (y-axis). The magnitude is only relative
within each property [18].
Newtonian Fluids
In the simplest type of flow, termed Newtonian, the material’s viscosity is constant and
independent of the shear rate [13][14]. That is, when shear stress (σ) is plotted against
shear rate ( γ& ) at a given temperature, the plot shows a straight line with a constant slope
that is independent of shear rate (see Figure 6). This slope is called the Newtonian
viscosity (η) of the fluid. The simplest constitutive equation is Newton’s law of viscosity:
σ = η ⋅ γ& [Pa] (Eq. 5)
From this it may be seen that a single point measurement, with a corresponding pair of
values of σ and γ& , would serve to rheologically define a Newtonian fluid.
All gases and common liquids such as ethanol, water and most oils are Newtonian. Also,
liquids with low molecular weight and solutions of substances with low molecular weight
in liquids, e.g. aqueous solutions of sugar or salt, are usually Newtonian.
fact that materials of this type, over a limited range of shear rates, correspond quite closely
to the model [24][28]. However, it ought to be noted that there are no fluids which behave
like an ideal Bingham material. This is only a generalized model to be used for non-ideal
Bingham materials [36]. For cement paste, there are disagreements as to which model best
describes the flow behaviour. These types of highly concentrated suspensions,
incorporating a high ratio of colloidal particles (i.e. particles smaller than approx. 1µm),
tend to show a more pseudo-plastic shear-thinning behaviour at equilibrium flow. In the
literature, different models have been proposed but the Bingham model and the Herschel-
Bulkley model tend to be best suited for cement pastes [25][28][34][37][38]. The Bingham
model is better suited for pastes with high water-to-cement ratio (w/c) than for those with
low w/c [25]. When superplasticizer is added, paste tends to show Newtonian behaviour at
low concentrations and viscoplastic behaviour at high concentrations [26]. SCC, however,
has been suggested to a have a shear-thickening behaviour with a yield, and the rheology
parameters are to be defined by the Herschel-Bulkley model (with A>1) [39]. Others
consider the apparent shear-thickening behaviour of SCC to be an artefact from the
experimental setup, caused by a lack of steady state during the measurement, where the
structure of flocculated colloidal particles has not been broken [40][41].
Typical values of yield stress and plastic viscosity for some cementitious materials, defined
by the Bingham model, are shown in Table 4. For SCC, it cannot be at the lower limits of
yield stress and viscosity simultaneously, since it would separate.
Table 4. Typical range of yield stress (σ0) and plastic viscosity (ηpl) for cement paste,
mortar, “normal” concrete (NC and flowing NC), and self-compacting concrete (SCC),
defined by the Bingham model [5] [19] [42].
Paste Mortar NC Flowing NC SCC
σ 0 [Pa]: 10−50 10−100 400−2000 100-400 10−100
η pl [Pa s]: 0.01−1 1−5 50−100 20-100 20−150
2a)
•
Shear rate, γ [1/s]
1) 3b)
2b) 3a)
•
Shear rate, γ [1/s]
Bingham
Some materials exhibit an infinite viscosity until a sufficiently high stress is applied to
initiate flow. Above this stress the material then shows simple Newtonian flow. The
simplest model covering these types of viscoplastic fluids with a yield response is the ideal
Bingham model, and is expressed by the following two parameter equation:
σ = σ 0 + η pl ⋅ γ& {σ > σ 0 } [Pa] (Eq. 7)
where ηpl is the model coefficient of plastic viscosity, and γ& is the shear rate. σ0 is the
constant which is interpreted as yield stress, and which often is referred to as the Bingham
yield stress or simply the yield stress of the material. The Bingham model can describe the
viscosity characteristics of a fluid with yield stress whose viscosity is independent of shear
rate, as shown in Figure 7. Therefore, the Bingham plastic model does not have the ability
to handle the shear-thinning characteristics of general non-Newtonian fluids.
Many concentrated particle suspensions and colloidal systems, such as mortar and
concrete, show Bingham behaviour at limited ranges of shear rate.
All rheological measurements presented in the appended papers (Paper I, II, III and VI), on
both mortars and concretes, were performed with the Bingham model.
Herschel-Bulkley
The Herschel-Bulkley model is a three-parameter model used to describe viscoplastic
materials exhibiting a yield response with a shear-thinning relationship above the yield
stress. It is a combination of Power-law and Bingham, and is expressed as:
σ = σ app + ηapp ⋅ γ& A {σ > σ app } [Pa] (Eq. 8)
where σapp is the constant that is interpreted as apparent yield stress, ηapp is the model
coefficient of apparent viscosity, γ& is the shear rate, and A is the model constant indicating
the degree of non-Newtonian behaviour (the greater the departure from unity, the more
σs
Load Respons
accuracy depends on the model used and the range and reliability of the experimental data
available. Several studies [14] have shown that a given fluid can be described equally well
by more than one model and, hence, can have different yield stress values.
It has been shown by many investigators that the empirical tests to some extent provide
information about the concrete rheology. Slump has for a long time been considered to be a
unique function of yield stress (Bingham), without influence by plastic viscosity [44]-[60].
More recently the horizontal flow spread, rather than the vertical slump, has been used to
calculate the yield stress [24][61]-[63]. Usually these correlations concern concretes in a
small range of flowability (e.g. HPC, SCC), and are not valid for other or wider ranges.
Often the correlation is purely empirical, but there are also some physical models proposed
to explain the relationship. The viscosity, on the other hand, is generally considered to
correlate with empirical tests recording the flow time. For SCC, this connection is usually
made with the slump flow spread time to 500 mm (T50) or V-funnel time [64]-[66].
In Paper I experimental results are presented, addressing the interaction between the slump
flow spread, flow time (T50), yield stress (σ0) and plastic viscosity (ηpl). It was shown that
the slump flow spread is not a unique function of yield stress, but rather a more complex
function of both yield stress and viscosity. However, the spread proved to be much more
closely related to the yield stress than to the viscosity, especially at high viscosity, whereas
the T50 time was connected more equally with yield stress and viscosity. These relations
are illustrated in Figure 10.
1000 1000
800 800
Slump flow [mm]
y = -124.65Ln(x) + 1071.82
600 2 600
R = 0.89
400 400
200 200
0 200 400 600 0 50 100 150 200
Yield stress [Pa] Viscosity [Pa s]
25 25
20 20
15 15
T50 [s]
T50 [s]
10 10
5 5
0 0
0 50 100 150 0 50 100 150
Yield stress [Pa] Viscosity [Pa s]
Figure 10. Measures of slump flow values vs. rheological parameters, individually, for
~550 mixtures with a wide range of consistency.
The following approximate models for calculating the relative slump flow area (Rp) and
the slump flow spread time T50 (in seconds) for flowable concretes (and mortars), over a
wide range of consistencies, was proposed:
( H / 6 )2
Rp ≈ (Eq. 9) R p = ( D / D0 ) 2 − 1 (Eq. 10)
ln( η pl + 2 ) ⋅ σ 0
T 50 ≈ 0.002 ⋅ σ 0 ⋅ η pl (Eq. 11)
where ηpl is the plastic viscosity, σ0 the yield stress, H the cone height (300 mm for
Abram’s cone), D the measured spread diameter in millimetres, and D0 the flow cone
bottom diameter (200 mm). The models are purely empirical and are deficient in units.
They are only intended to roughly illustrate the interaction between the rheological
parameters and slump flow values.
In the literature it is not generally agreed that slump flow is a unique measure of concrete
yield stress [67]-[73]. It has been noted that the correlation is weak, or that relation
between yield stress and slump flow, without taking viscosity into account, does not show
a satisfactory fit. In Figure 11, typical values for SCC, presented by Nielsson and Wallevik
[67], are plotted in the diagram from Paper I showing the correlation between the
measures of slump flow values and rheological parameters.
120 550 mm 600 mm 650 mm 700 mm
>700 mm
600-700 mm
90 500-600 mm
Yield stress [Pa]
500-600 mm
60
30 600-700 mm
>700 mm
0
0 50 100 150
Viscosity [Pa s]
Figure 11. The slump flow spread (mixtures with a spread <500 mm are excluded) and
Bingham rheology parameters (yield stress and plastic viscosity) for SCC from Paper I,
complemented with typical values for SCC from [67].
It should be noted that these changes are purely time related and the materials flow
characteristics need to be studied as well. It is possible that a material could be both
thixotropic and shear-thickening or shear-thinning.
In order to characterize the rheology of cementitious materials and other time-dependent
material, one has to be aware of these effects. It is necessary to study the time dependence
of the material in order to design a conditioning regime. To be able to compare
measurements in common references, it is important to take steps to pre-condition the
sample. The best method for this purpose is to pre-shear the sample for a time sufficient to
destroy any structure (flocculated colloidal particles) [41]. One way to do this is to start at
a high shear rate for a sufficient time, followed by measuring stress while decreasing the
strain rate from high to low. Another method is to initiate each measurement with a
constant shear, applied for a time sufficient to reach equilibrium (within acceptance)
[14][28]. At low strain rates a suspension may be very slow to reach equilibrium.
There are many methods proposed, based on rheological measurements, for how to
characterize the time dependence. However, the quantification of thixotropy in absolute or
fundamental terms is problematic, as it depends on the shear history of the material as well
as the method used to measure and evaluate the thixotropy; hence the thixotropic value is
often only relative. A commonly used technique to determine the thixotropy is to measure
the time needed for a structural breakdown [28]. This is usually done by applying a
constant shear rate (or stress), and recording the time for the measured shear stress (or rate)
to reach an equilibrium state (within acceptance); see Figure 14. As the breakdown time
depends on the size of the applied shear, the test can be performed at different specific
levels of rate (or stress), respectively. A method to characterize the material’s thixotropy
with a single value [76][77], when using different levels of shear, is to determine the area
between the curves of initial shear stress and equilibrium shear stress (see Figure 13).
Shear stress, σ [Pa] Shear stress, σ [Pa]
Equilibrium
shear stress
•
Time, t [sec] Shear rate, γ [1/s]
Figure 13. Thixotropy represented by the evaluated area between the curves of initial
shear stress and equilibrium shear stress
Another popular method, especially for cementitious materials, is to quantify the time
dependence by the area of a flow hysteresis. This area represents the energy needed to
break down the structure [78]. In a typical rheometric test, shear stress or shear rate is
ramped at a fixed speed up to a maximum value, then ramped back down at the same speed
to the beginning (see Figure 14). In hysteresis, one flow curve lies above the other,
forming a continuous loop whose internal area depends on the shear and thermal history of
the material, and on how rapidly the stress or shear rate was ramped. Not all researchers
agree that the area of a flow hysteresis in measurements of stress as a function of rate
represents any material characteristics. The first method, where the stress is measured
directly as a function of time at some strain rate, is considered to better reflect the
thixotropic behaviour [28].
Shear stress, σ [Pa] Shear rate, γ [1/s]
• •
Thixotropic
area [Pa/s]
Shear stress, σ [Pa]
Thixotropic
time [s]
•
Shear rate, γ [1/s]
Figure 14. Thixotropy quantified by the area of the flow hysteresis when the shear rate is
ramped up and down, or alternatively by the time to steady-state (equilibrium) flow at
constant shear rate.
In Paper II, a thixotropic measurement on mortars was performed, using the latter method
with the area of the flow hysteresis.
There is no general agreement that the thixotropy can be evaluated by measuring structural
breakdown, nor that methods based on the calculated area represent any material
characteristics [28]. The structural build-up at rest, rather than the breakdown, is proposed
to better represent the material’s true thixotropic behaviour [29], and it is to be monitored
without breaking down the structure. Furthermore, the elastic region of a viscoelastic
material is proposed to represent the structure; hence it is to be characterized by a strain-
stress measurement where the structure corresponds to the peak stress (the static yield
stress), just before the material’s elastic structure breaks and turns into a plastic state (see
Figure 8). However, it can be problematic to avoid a structural breakdown when
measuring this peak level. Moreover, the peak level is dependent on the applied rate of
shear strain (or shear stress when measuring the strain).
Another non-destructive method to measure the material’s structure, represented by its
elastic region, is by an oscillating rheology test. The deformations are small and kept
within the linear viscoelastic region, so the structural build-up can be monitored over a
time period without destroying the structure. In a typical oscillation test, illustrated in
Figure 15, the applied periodic stress (σ) and the resulting strain (γ) can be described as:
σ = σ 0 ⋅ cos( ω ⋅ t ) [Pa] (Eq. 12) γ = γ 0 ⋅ cos( ω ⋅ t − δ ) [-] (Eq. 13)
where σ0 is the stress amplitude, γ0 is the strain amplitude, ω is the angular frequency, t is
the time, and δ is the phase lag (loss angle) [14][79]. For an ideal solid the phase angle will
be δ=0, whereas for a Newtonian fluid with a purely viscous response it will be δ=2π
(=90°). The materials rheological characteristics are described in terms of the shear storage
modulus G’ (representing the elastic response of the material), and the shear loss modulus
G” (representing the irreversible viscous response) can be calculated as:
G' = σ 0 / γ 0 ⋅ cos( δ ) [Pa] (Eq. 14) G" = σ 0 / γ 0 ⋅ sin( δ ) [Pa] (Eq. 15)
Strain, γ [-]
Stress, σ [Pa] Phase angle, δ [rad]
σ0
γ0
Time, t [sec]
There is no general agreement that the true Yield stress, σo and σs [Pa]
thixotropy can be evaluated by measures of Static yield stress (σs)
structural breakdown, but rather methods using Thixotropic
structural build-up at rest are to be used [29]. This area [Pa·s]
Dynamic yield
is proposed to be characterized by a non- stress (σo) Reversible
destructive method, for example by the peak stress structure
(see Figure 8) in a strain-stress measurement [29].
To exclude the time-dependent irreversible Non-reversible
structure
behaviour from the reversible (thixotropic), the
static yield stress is to be related to the dynamic Time, t [sec]
where A is a constant, E0 is the fluid activation energy in J/mol, R is the gas constant, and T
is the absolute temperature in Kelvin. For water at 20°C, the equation can be
approximately written as:
η = 5.5 ⋅ e ( −2520 / T ) (Eq. 17)
To maintain ±1% accuracy in the measurements of viscosity, at 20°C, the sample then
must hold the temperature to ±0.3°C. For particles suspended in water, the viscosity rises
with concentration and the temperature dependence increases. Consequently, precise
control of the sample temperature is necessary to measure viscosity accurately.
The measuring techniques can be divided into four principal ones, as shown in Figure 17.
Rheometers
Figure 19. Rheometers’ principal techniques for determining the viscosity and yield stress.
Most of these rheometers can produce viscosity measurements at a specified, constant
shear rate or shear stress (normally a constant shear rate is applied). Therefore, in order to
measure the viscosity over a range of shear rates, one needs to repeat the measurement by
varying either the pressure in the reservoir tank of the capillary-tube rheometer, or the
rotating speed (or torque) of the cone or cup in the rotating rheometers. In addition, since
these tests are to be performed at a stationary state, the capillary-tube rheometer is not very
applicable to a thixotropic fluid like fresh cementitious materials where the samples are to
be pre-sheared before measuring. For the yield measurement of viscoplastic materials, the
indirect methods are preferred rather than direct methods, for practical reasons [43]. Thus,
the direct methods will not be rigorously discussed.
In a rotational rheometer, the fluid sample is sheared as a result of the rotation of a cylinder
or cone. The shearing occurs in a narrow gap between two surfaces, usually one rotating
and the other stationary. Three frequently used geometries are: the coaxial (concentric)
cylinder, the cone-and-plate, and parallel plates. The coaxial cylinder is the most
commonly used [14].
In a capillary-tube rheometer, the fluid is made to flow through a capillary tube and the
rates of flow under known pressure differences are measured. This method is commonly
used in the process industry, where the apparatus can be installed in series with the flow.
Standardized measuring geometry for the different rheometers can be found in DIN 53018,
DIN 53019, ISO 2884 and ISO 3219.
For particle suspensions, such as cementitious materials, there are well-established rules
for the geometry of apparatus and sample to ensure that rheological measurements are
reliable. The chief rules are that any dimension should be at least 10 times the size of the
largest particles (Ro-Ri≥10·Dmax) and that the ratio of outer to inner cylinder radius should
be less than 1.2 [14][19][28]. It can be noted that this is not the narrow gap that is required
to generate a known shear profile (Ro/Ri≤1.01), but in order to have manageable
equipment the maximum ratio of radii is set to 1.2 without generating too large errors. E.g.
if 0.5 mm particles and a narrow gap are to be used, the diameters of the inner and outer
cylinders would have to be approximately 1 metre. Wide-gap (Ro/Ri>1.2) concentric
cylinder rheometers exist, but the calculation of shear stress and rate requires broad
assumptions concerning these parameters over the range of shear across the gap. Thus,
small-gap (Ro/Ri≤1.2) rheometers are preferable because they do not require large
assumptions, and they also decrease the risk of plug flow [20][26][28].
For a viscoelastic fluid, at low shear rate, there is always a risk of plug flow. If the shear
stress falls below the yield value (see Figure 22). The velocity gradient over the profile
will change, and there will be a part of the material without velocity. The gap where flow
occurs will then be reduced to an indeterminable value, so the calculations of angular
velocity and torque into shear rate and shear stress will not be valid. With a rotating inner
cylinder, the plug of solid material will appear at the outer cylinder and at the inner
cylinder when the outer is rotating. In a flow curve (shear rate versus stress), plug flow will
be manifested as loss of shear stress in the low shear rate region. For a Bingham fluid, the
measured values at low shear rates will diverge from the linear curve (similarly to the non-
ideal Bingham-plastic behaviour in Figure 6, curve 3a); hence these values are to be
excluded. The lower limit of the angular velocity (Ω), where all material is sheared in the
gap, for a Bingham fluid, can be calculated as [28]:
For mortars and pastes, the grooved inner cylinder and the vane have been shown to
provide stable measurements and equal results, whereas the smooth (conical and concave
in Figure 21) gave deficient measurements with a shear-thinning behaviour (indicating
wall-slip) and with a larger scatter.
Lubricating slip-layer
Ro
”plug” Ω
Ri
Ω
Complete Incomplete
flow flow
Shear stress σ
σ < σ0
γ·
Shear rate
(velocity)
Figure 22. Illustration of plug flow, with a Figure 23. Illustration of wall-slip, with a
section of solid material at the outer lubricating slippage layer of suspending
cylinder (when the inner rotates), where media formed at the surface of the inner
the shear stress is below the yield value. cylinder.
For cementitious materials, the concentric (coaxial) cylinder is the most commonly used
system for rheological measurements, usually with some type of grooved or ribbed surface
on the inner or outer cylinder (or both). Also the vane type is commonly used for
cementitious materials. A well-known commercial apparatus using this system is the BML
rheometer for concrete. In the appended papers, the rheological measurements on mortars
and concretes were performed using a concentric system.
∆P
2·R
3 EARLY-AGE DEFORMATION
3.1 Introduction
When a porous body loses water to the ambience, contraction will take place. For
cementitious materials there will also be an additional shrinkage caused by the chemical
reactions (hydration, carbonation, etc.). Since the rigidity, as well as the effect of different
chemical reactions, changes with time, it is convenient to distinguish between early-age
and long-term behaviour, where early age is limited to 24 hours from mixing and long-
term refers to the time beyond. However, there is not a well-defined and distinct transition
but rather a continuous transformation from a plastic to a rigid state. Shrinkage of a
cementitious material will start as soon water is added, due to the chemical reaction and
also due to the loss of water by evaporation (if not prevented). In the initial fresh state,
when the concrete is still a fluid, the volumetric shrinkage will, fully or partly, result in a
vertical displacement (settlement) [81][82]. This deformation does not result in any
stresses and is often ignored in the design of concrete structures, since it is considered to be
less than the subsequent deformations or is considered not important. Moreover, in the
fresh state, shrinkage measurements are difficult to perform without involving the effect of
gravity (bleeding, segregation, etc.) which, in addition, is not isotropic.
Yet in order to elucidate the mechanism of early-age deformations, and in view of the fact
that they are greatest up to an age of 12 hours, these deformations should be investigated
and may have to be taken into account. The governing mechanisms of the total shrinkage,
distinguishing between early age and long term, are illustrated in Figure 27. It ought to be
noted that there are also structural and environmental factors that simultaneously can cause
expansions, e.g. alkali silica reactions, delayed ettringite formation, expansive cements,
sulphate attack, thermal changes and reabsorption of water. There is generally an interplay
between the mechanisms of contraction and expansion, but often the contracting part is
predominant. However, the mechanisms of expansion have not been considered in this
work. Neither are the long-term deformations further explored.
Total shrinkage
Early age (<24 hours) shrinkage Long term (>24 hours) shrinkage
Figure 27. Illustration of the driving mechanisms of the total shrinkage, not considering
the mechanisms of expansion, or including the structural restrain.
Shrinkage, especially at early age, has become of great concern, due to recurrent problems
with cracking in concrete structures. Conditions such as reduced maximum aggregate size,
increased amount of fines, presence of retarding admixtures, increased binder content, and
deficient covering and curing all contribute to these problems. In recent research there has
been a growing interest in the area of autogenous and plastic shrinkage, as well as how to
control and counteract the early-age shrinkage. A “hot topic” today is e.g. the use of
superabsorbent polymer for internal curing [83]-[88].
There are two main driving forces for early-age shrinkage [81]: (1) evaporation shrinkage
(or early-age drying shrinkage) due to loss of water from the fresh concrete, and (2)
shrinkage due to hydration and chemical reactions producing autogenous shrinkage. Yet
under sealed conditions, if evaporation is prevented, the early-age shrinkage is a result of
the autogenous shrinkage. However, temperature dilation may also contribute (e.g. when
cooling the surface), as well as the external suction of water (absorption) by the formwork
material or by the sub-base. Accordingly, cracking in the initial phase is a product of
several factors. Thus, it is important to separate the mechanisms into those that are
dependent on environmental conditions (e.g. evaporation of water from the surface) and
those that occur without moisture transfer to the ambient and which are associated with the
autogenous deformation of the material.
The term “plastic shrinkage” refers to the periods (1 and 2) until the point of final set
[22][23][89]. However, neither the initial nor the final set is a distinct and well-defined
physical state, but merely a gradual change of structure due to hydration. The points of
setting are often arbitrarily chosen, referring to measures from empirical methods. As the
point of final set is arbitrarily determined, so is the period of plastic shrinkage. However,
this period is often simply given a general time (e.g. 12 or 24 hours). Commonly used
methods for determination of setting (initial and final) are the Vicat needle method (EN
196-3) and the penetration resistance method (ASTM C403). There are also ultrasonic
techniques proposed for better prediction of setting time [92]-[94].
Final set
ettringite formation
Rapid formation Diffusion-controlled
of C-S-H and CH reactions
Induction period: Formation of
increase in Ca2+ monosulfate
concentration
Initial set
I II III IV V
~10 minutes ~4 hours ~12 hours ~24 hours Time of hydration
~2% ~15% ~30% Degree of hydration
Figure 30. Schematic representation of heat evolution during hydration of cement and
water, based on Gartner et al. [101].
In Figure 31, the products associated with the stages of cement hydration and the change
of porosity and permeability can be seen. The setting process is the consequence of a
change from a concentrated suspension of flocculated particles to a viscoelastic skeletal
solid capable of supporting an applied stress; see Figure 32. Setting is controlled primarily
by the hydration of C3S and occurs when the induction period is terminated by a rapid
hydration of C3S leading to a fast temperature rise of the concrete (Stage III) [22].
However, not only the w/c ratio will influence the hydration, but also a number of
parameters such as: the composition and fineness of the cement (the main clinker
components); addition of supplementary materials (such as fly ash and silica); admixtures
(super plasticizer, accelerator, retarder, etc.); and the temperature.
Concentrated suspension Formation of a layer of Nucleation and early Rapid formation of ‘C-S-H’
of flocculated particles ettringite or ‘AFt’ and formation of ‘C-S-H’. leading to solidification and
‘CH’. Possible particle Continued formation of creation of capillary pores
agglomeration ‘AFt’. Particle agglomeration
cement
water
cement ~25% of its initial volume is lost, and 1 gram of cement will consume 0.23-0.25
grams of water when fully hydrated. Hence, the chemical shrinkage amounts ~6 ml per 100
gram of cement reacted.
The basic reactions of cement clinker are generally defined by four reactions of C3S, C2S,
C3A and C4AF. Each of these reactions requires water, is exothermic, and results in a
different decreased volume of the reaction products [97]. The contribution from each of
these four phases to the chemical shrinkage is given in Table 5.
I. Placing/casting
Chemical
shrinkage
Chemical
II. Initial set shrinkage
Shrinkage
Empty pores
Chemical
III. Hardening
shrinkage
Initial set
Autogenous shrinkage Autogenous
shrinkage
Time Hydration products Cement Water Empty pores
I. II. III.
Figure 33. Principle of autogenous and chemical shrinkage for a cement paste under
sealed conditions.
As mentioned, the chemical shrinkage begins immediately when mixing cement and water
and the rate of shrinkage is highest during the first hours. Chemical shrinkage is suggested
to be almost linearly proportional to the degree of hydration (except for the very initial
hydration) [105][106]. It has also been shown that the chemical shrinkage correlates
linearly with the strength development, once the paste has set [107]. Factors such as
temperature, w/c, cement fineness, C3A and C4AF content, and the efficiency of cement
dispersion will have a significant effect on the rate [23]. Also additives such as chemical
and mineral admixtures and pozzolans will influence the chemical shrinkage [22].
which reflects the difficulties in the interpretation of the results based on different
techniques [81][111][123].
The pattern of autogenous deformation, exemplified in Figure 34, comprises three distinct
stages which can be defined as: (1) plastic, (2) semiplastic and (3) rigid, separated by the
time to initial and final set [91]. In literature, other terms for these stages can be found, e.g.
liquid / skeleton formation / hardening [89]. Also the four stages: initial / induction /
acceleration / deacceleration, connected with the chemical reactions, can be found [125]. It
has been suggested [81] that, when measuring the autogenous shrinkage, the setting (initial
and final) will be manifested as a change of the slope of the deformation. Initially the
autogenous shrinkage originates from the chemical shrinkage, whereas once the concrete
sets the development of a contracting capillary pore pressure will contribute to the
subsequent deformation (see Figure 34) [116].
Plastic Semiplastic Rigid
Initial set
Final set
Temperature (measured)
0 6 12 18 24 0 6 12 18 24 0 6 12 18 24
Autogenous deformation [10 m/m]
0 0 0
-6
-6
w/c 0.55 -200 40% (8-16)
-400 0% Silica -200
5% Silica 30% (8-16)
-400 10% Silica 20% (8-16)
-800 -400
w/c 0.45 -600
w/c 0.38
2% SRA
-6
Ref.
0.8% SP -200
-200 -200 1% SRA Retarder
1.0% SP 0% SRA
-400
-400 -400
-600
Since the fluid pressure is less on the convex side of a meniscus than on the concave side,
the creation of water menisci results in a negative pressure in the pore water and
contraction forces between particles [4]. Consequently, the average distance between the
particles tends to be reduced and the paste contracts [9]. These contracting capillary forces
are in inverse ratio to the meniscus radius, and hence the capillary tension stresses increase
with decreasing pore sizes and interparticle spaces (e.g. with low w/c, high cement
fineness, additions of fines, etc.). For a concrete where evaporation is prevented, a negative
capillary pressure will also start to develop, but only once the hydration commences and
the concrete sets [89]. As a solid skeleton starts to form the chemical shrinkage is not
totally transformed into external volume change and, if the water supply is restricted,
empty pores will be formed inside the paste, and contracting water meniscus are created
(see Figure 33 and Figure 34). At the stage where the concrete starts to set (initial set) both
the capillary pore pressure and the temperature reaches an accelerating phase (see Figure
34 and Figure 37), which indicates that the dormant period is ended and that the cement
hydration accelerates [91]. Initially (before setting), when the concrete is liquid-like,
without restraining skeleton and empty pores, the pore pressure is zero [116]. According to
Wittman [9] the action of capillary pore pressure the cause of plastic shrinkage.
Typical development of pore pressure is shown in Figure 37. As can be seen, the pore
pressure develops more rapidly in an evaporating concrete than in a sealed one. The
accelerating phase of pore pressure starts at 5-6 hours from mixing for a sealed concrete,
whereas for an evaporating one it accelerates at 3-4 hours [91]. It can also be noted (in
Figure 37) that the initial cracking, due to plastic shrinkage, which coincides with the
accelerating phase of the pore pressure (3-4 hours from mixing). Furthermore, a pressure
close to the exposed surface is ahead of a lower pressure. However, for SCC’s with a high
w/c (>0.55) these differences are smaller, and for standard concrete the pressure at the
different distances from the surface will develop almost equally in time [91]. This can be
explained by the concrete’s ability to transport water to the surface in relation to the
evaporation [116]. Thus, for a denser and less permeable matrix the internal transport of
water to the area close to the surface, having a larger capillary tension (due to evaporation),
will be restricted. Whereas for a more porous and permeable matrix the balancing of the
differences in pore pressure, and the transport water to the surface, will be faster and the
pressure will be more uniform through the section.
Max Max
Temp.
Figure 37. Typical measurementss of pore pressure and temperature development, for a
SCC with w/c 0.55. To the left, pore pressure and temperature together with the
autogenous deformation, and to the right with the strain and evaporation (ring test). The
axes have been normalized against maximum and minimum values.
The capillary pore pressure (Pc) that is generated can be described by the Gauss-Laplace’s
equation (Eq. 19) which relates the pressure to the capillary radius, and by the Kelvin’s
equation (Eq. 20), which relate the pressure to the relative humidity (RH). The capillary
pore pressure is, by definition, the differences between the pressures in the fluid that lies
on the concave side of the surface (in this case the air pressure, Pa) and in the other fluid
(in this case the water pressure, Pw) [116]; see Figure 36.
2 ⋅γ w ⎛1 1⎞
Pc = Pa − Pw = − = −γ w ⎜⎜ + ⎟⎟ [Pa] (Eq. 19)
r ⎝ r1 r2 ⎠
2 ⋅γ w ⋅ M w 2 ⋅γ w ⋅ M w ⎛ 1 1 ⎞
ln(RH ) = − =− ⋅⎜ + ⎟⎟ [-] (Eq. 20)
ρw ⋅ R ⋅T ⋅ r ρ w R ⋅ T ⎜⎝ r1 r2 ⎠
where γw is the surface tension of the capillary water (~0.074 N/m); r is the mean curvature
of the surface; r1 and r2 are the principal radii of curvature in metre (see Figure 39, R is the
ideal gas constant (8.314 J/mol K); T is the absolute temperature in Kelvin (20°C≈293K);
Mw is the molar mass of water (~0.018 kg/mol); and ρw is the density of water. By
combining the two equations, and setting Pa equal to zero (= atmospheric pressure) and r1
equal to r2, the following relationship is obtained:
ρw ⋅ R ⋅T
Pc = ⋅ ln(RH ) [Pa] (Eq. 21)
Mw
This equation (Eq. 21) shows that a small 1 000 000
reduction in RH will lead to very large Capillary pore pressure [kPa]
100 000
capillary pressure; see Figure 38. Yet, the
pressure can only develop if there are partly 10 000
empty pores available in the system. Once 1 000
the matrix sets and the pores lose their
100
internal water (by hydration, evaporation,
etc.) the pores loses their internal water, 10
starting with the largest pores, and RH will 1
start to drop [100]. In addition, the 0 0.5 1
dissolution of salts into the pore water will Relative humidity, RH [-]
increase the alkalinity (i.e. concentration of
OH- ions, mainly from KOH and NaOH) and Figure 38. Relation between RH and
consequently reduce the RH. This reduction capillary pore pressure (at 20°C),
will be 1-3%, depending on the cement based on the Kelvin equation. Note,
composition and w/c ratio [126]. pressure is negative and logarithmic.
Based on the assumption that the capillary pores in the paste are typically in the size range
of 0.01 to 5 µm [90], the pore pressure calculated with Kelvin’s equation (Eq. 20) will
roughly be in the rage of -10 kPa and -10 MPa. If the gel pores, down to 2 nm [99], were
included, the pore pressure would theoretically be as low as -100 MPa.
r1
r1
r2 r1 r2 r*2 r*2
r1
∆Pc
Figure 39. Schematic representation of liquid filled joint between two spherical particles
at the surface.
According to Powers [4] the maximum negative capillary pore pressure, Pc,max, developed
in a cement paste mixture is indirectly proportional to the w/c:
γw ⋅S
Pc ,max = −1 ⋅ 10 3 ⋅ [Pa] (Eq. 22)
wc
where S is the mass specific surface area of the cement [m2/kg] measured with Blaine.
Assuming S = 350 m2/kg, and w/c ratio 0.55, the capillary pressure calculated with
equation (Eq. 22) will be -45 kPa, in a fully hydrated cement paste. However, this is not
near the theoretical lower limit of -100 MPa [128] in the smallest pores in the gel.
Many factors have an impact on the pore pressure development, related to the evaporation
as well as to the hydration. That the rate of hydration (apart from the rate of evaporation)
plays an important role for how the capillary pressure develops is shown in Figure 40,
where concretes with accelerator and retarder, and with different superplasticizer dosage,
change the time of the pressure drop. It should be noted that the time to, and magnitude of,
maximum underpressure are often not possible to evaluate, due to a collapse (loss) of
measured pressure at random times. This effect is usually referred to as the breakthrough
pressure [9][116], and is the effect of air penetrating the pressure transducer, as the
surrounding water menisci cannot find stable positions in the region adjacent to the
measuring point.
0 0 0
-20 -10
Accelerator -40
-40 Ref. -20 1.0% SP
-60
0.6% SP
Retarder
-60 -30 -80 Evaporating
0.8% SP Sealed
-100
-80 -40
0 2 4 6 8
0 2 4 6 8 0 2 4 6 8
Time (from mix) [hours] Time (from mix) [hours] Time (from mix) [hours]
This pressure, called disjoining pressure, will rise with an increase in RH of the system and
lead to an expansion. Consequently, when the system dries out and RH is reduced the
particles will contract [129][130]. The disjointing pressure concerns aggregations in which
the smallest interparticle distance is much smaller than the particles [4], and is active in the
area of hindered absorption where the distances between the surfaces are smaller than two
times the thickness of free adsorbed water layer (~20Å at 100%) [22] [130]. The
disjointing pressure develops steady in the range between 100% and around 40% [131],
and shows an RH dependency similar to the capillary stress. It increases with increasing
thickness of the adsorbed water between the particles (i.e. increased RH) until it exceeds
the van der Waals’ attraction, when the particles will be forced apart. Therefore, on first
drying and lowered RH, the decreasing disjoining will case the particles to be drawn
together by the van der Waals’ forces, and there will be net volume shrinkage [22].
However, there is not a general agreement that the disjointing pressure has a significant
influence on the autogenous shrinkage of cementitious materials [125].
4 30
Water Sealed
25
w/c 0.55
2
w/c 0.45 20
1 w/c 0.38
Evaporatin
0 15
0 6 12 18 24 0 5 10 15 20
Time [hours] Time (from mix) [hour]
Figure 42. Example of evaporation from Figure 43. Temperature development for
SCC with w/c from 0.38 to 0.67, exposed to a sealed SCC (w/c 0.55) exposed to air
air with 4.5 m/s, 35% RH and 23°C. at 4.5 m/s, 35% RH and 23°C [91].
in contact with the cement paste sample. Bovin et al. [106] have shown that there is a high
correlation between the two ways of measuring.
The dilatometric method was initially developed by Le Chatelier [138] . This method
consists of immersing a given mass of cement paste in a glass flask, e.g. of “Erlenmeyer
flask” type, filled with water and surmounted by a graduated capillary tube (see Figure
45). The flask is to be placed in a thermostable bath at constant temperature (usually at
20°C). The decrease in volume of water, gradually consumed by the hydration reaction, is
manually read on the capillary tube at regular intervals [139].
The buoyancy method is based on the same principles as the dilatometric method, but
instead of following the volume of consumed water directly, the sample’s reduced
buoyancy is recorded (see Figure 45). Based on Archimedes’ principle, the water
submerged sample will register a volume reduction by weight [106][136][140][141]. An
advantage of this method is that the reading can be logged.
Thermo stable bath
0.001 g Balance
Graded tube
Plug Cup
Flask Membrane (oil)
Water Water
t Cement paste Cement paste
l0
l0
to gas) will also contribute to the total deformation. Moreover, the plastic shrinkage is only
a relative measure as it strongly depends on a number of factors related to the sample’s
geometry and environmental conditions [23]. Thus, these factors are to be controlled and
well defined. Methods proposed for plastic shrinkage measurements (e.g. ASTM
C157/C157M and C426) need a certain level of rigidity in order to measure the shrinkage,
and usually do not consider the deformation during the first 24 hours after casting [118].
For early-age plastic shrinkage, measurement is to be started prior to demoulding. For
concrete, a method has been proposed [145][152][153] for measuring the linear plastic
shrinkage on slab-type samples in a rigid mould. This is performed analogously to the
linear autogenous deformation, but the top surface is exposed to drying at controlled
ambient condition (air velocity, RH and temperature). As the material must have some
degree of rigidity, tests are complemented with a transducer recording vertical
displacement (settlement). By simultaneously measuring the vertical and horizontal
displacement, the volumetric shrinkage can be calculated for the whole period of early-age
shrinkage. Furthermore, complementary measurements of weight loss can be recorded by
placing the sample on a balance, in order to evaluate the evaporation (see Figure 49).
Displacement
Measuring rod
Low friction surface transducer (vertical) Fan
Mould (e.g. teflon foil) Thermo couple
Displacement v, T, RH
transducer
Figure 49. Principle of linear plastic shrinkage measurement on a slab exposed to drying,
with displacement transducers recording the vertical and horizontal deformation.
4 EXPERIMENTAL WORK
4.1 Introduction
Complementary information concerning the experimental methods and materials used in
the appended papers is presented in this chapter. Further, a more detailed description is
provided, and some further analysis of the methods and the results is made.
In Paper I the influence of Bingham rheology parameters on the slump flow values of self-
compacting concrete and mortar is evaluated, and it addresses the complex connection
between the slump flow spread, flow time (T50), yield stress and plastic viscosity. A large
number of more or less self-compacting mortars (~200 mixtures) and concretes (~550
mixtures) with a wide range of consistency were used. The mortar rheology was measured
by using a Bohlin CVO200 rheometer with concentric setup, and for concrete a ConTec
Visco5 rheometer was used.
In Paper II the properties of eight different fillers (seven limestone and one glass filler)
and their influence on the rheology of self-compacting mortar are evaluated. The mortar
rheology and slump flow were measured using the same setup as in Paper I. Traditional
methods for determining the surface area of filler material were used, such as the area from
size distribution (laser diffraction), by image analysis (SEM), Blaine, and by BET(N2). In
addition, a simplified method called BET(H2O) was used. Geometrical properties such as
F-shape, F-circle and Compactness were determined from image analysis (SEM), and the
fillers’ retained water ratio and deformation coefficient were measured.
In Paper III the effect of the specific surface area of gravel and limestone filler on the
rheology of self-compacting concrete is evaluated. The area was measured with the
BET(H2O) method, as in Paper II. The differences in BET-area were used as a basis for
calculation of the water demand for the concrete mixes. The concrete rheology and slump
flow were measured using the same setup as in Paper I. The mix design and its
constituents comprised typical materials and compositions for SCC in Sweden. A 0-8 mm
natural gravel, collected at five different occasions, was used, as well as five limestone
fillers with different geological origins.
In Paper IV the influence of fineness of concrete constituents on early-age (<24 h)
autogenous shrinkage is investigated. The experiments were conducted on SCC,
incorporating the same five limestone fillers as in Paper III. Tests were also conducted on
corresponding mixes without cement, i.e. without chemical shrinkage. A newly developed
concrete dilatometer was used, generating measurements of linear autogenous (sealed)
deformation of the concrete cast in a vapour-proof flexible tube mould. Temperature and
pore pressure were simultaneously measured on the sealed samples together with the
deformation.
In Paper V the influence of mix design on autogenous deformation (with the same method
as in Paper IV) and crack tendency due to plastic shrinkage are evaluated. For the crack
tendency test, a modified ring-test method was used where the concrete specimens were
exposed to early drying conditions while restrained by an inner steel ring. A large number
of different SCC constituents and mix compositions were investigated: e.g. w/c-ratio from
0.38 to 0.67, silica fume, and different admixtures. For comparison, tests with standard
concrete were also made.
Paper VI summarizes Papers II-V, with the focus on the five limestone fillers with
different BET-area and their effect on the fresh and hardened properties of self-compacting
concrete (SCC). Complementary tests of compressive strength (28 d) were made.
Figure 51. Pictures of limestone fillers, taken with SEM. The pictures edge length
corresponds to 0.5 mm. To the left, the relatively coarse “L70” filler with a large specific
surface area. To the right, the “L40” filler which was used as a reference.
Compactness
3 400
J 1.0 F-shape 65 000
3
I 0.9 Surface area
2
BET(H2O) [m /kg]
3 000
60 000
2
G 0.8
2 800
0.7
2 600 55 000
2 400 0.6
Figure 55. Photo showing the mixers. To the left is the Hobart mixer used for the mortars,
and to the right the BHS mixer used for the concretes.
A Size distribution
S size = = 50
ρ ⋅V m4
6 ∑ ( mi ⋅ d i )
40
2
Staying [weight-%]
The size distribution from the image analysis (SSEM) was determined according to the
Nordtest method NT BUILD 486, a method based on measurements of the maximum Feret
diameter (Fm) of 2D intersected 3D particles, where the total number of 2D objects per
unit area in size class i (nai) is calculated as:
k
nai = ∑ p j ⋅ n j ⋅ H j [pcs/m2] (Eq. 25)
j =1
where k is the number of classes and pj is the probability that a 3D particle of size H j will
be observed as a 2D object in size class i. nj is the number of 3D objects and H j is the
geometrical mean size in class j.
The SSEM was calculated, assuming cubical particles (shape factor 0.668) with uniform
density (ρ), as [4]:
6 ∑ ( Dcircle,i )
2
A
S SEM = = ⋅ [m2/kg] (Eq. 26)
ρ ⋅ V ρ ∑ ( Dcircle,i )
3
where Dcircle is the diameter of a circle with the same area as Area, A
measured (see Figure 57), and was computed as:
Dcircle = 2 ⋅ A / π [m] (Eq. 27) Dcircle
Even though the laser diffraction and the scanning electronic microscope (SEM) recorded
relatively small particles, the calculated area was still 10 to 100 times smaller than the area
measured with the BET method. This proves the significance of the particles’ shape,
porosity and texture of the surface area. Furthermore, in Paper II it was shown that the
correlation between the specific surface areas from size distribution (Ssize and SSEM) and by
BET was poor, whereas the correlation with Blaine was strong. The relationship with the
rheology measures was also poor.
The results, presented in Paper II, show that the effect of specific surface area by BET(N2)
for different filler materials on the mortar’s rheology was significant, and that the BET-
area (with N2 as well as with H2O) was the parameter that corresponded best to the
rheological parameters.
y [kg/kg]
coverage), C is a constant related to the
heat of adsorption, and u is the moisture b
content (i.e. the weight of the adsorbed gas) a
defined as: 0.113 0.331
RH [-]
(m − mdry )
u= [kg/kg] (Eq. 29)
mdry Figure 59. BET-plot with the
intersection point (a) and slope (b)
where m and mdry are the sample weight in calculated from the linear relation-ship
adsorbed and dry condition. between y and RH.
By using a so-called BET-plot (see Figure 59), where the adsorption isotherm (y) is plotted
against RH, a linear relationship is created with the intersection point (a) and slope (b) as:
y = a + b ⋅ RH [kg/kg] (Eq. 30)
RH
y= [kg/kg] (RH {0;1}) (Eq. 31)
u ⋅ ( 1 − RH )
1 ( C − 1)
a= [kg/kg] (Eq. 32) b= [kg/kg] (Eq. 33)
xm ⋅ C xm ⋅ C
From this BET-plot, a and b can be determined (graphically or by linear regression), and
the two unknowns xm can be derived as:
1
xm = [kg/kg] (Eq. 34)
a+b
The specific area (S) is directly proportional to the amount of monomolecular adsorbate, as
[156]-[157][160]:
xm ⋅ N
S= ⋅ Am [kg/kg] (Eq. 35)
M
where N is Avogadro´s number (6.022·1023 molecules per mol), M is the molecular weight
of the adsorbate (for water 18.016·10-3 kg per mol), and Am is the area occupied per
molecule of adsorbate in a monolayer. For water, Am is approximately 10.6·10-20 m2 per
molecule [26][156][127][159]. As a perspective, one litre of water in one molecule layer
will cover 3,546,000 m2. From this, the specific surface area by BET, with water as
adsorbate, can be calculated as:
3.54 ⋅ 10 6
S BETH 2 O = [m2/kg] (Eq. 36)
a+b
It should be noted that adsorption is not the same for moisture as for nitrogen gas. The
water molecule is smaller than the nitrogen molecule (10.6 Å2 for water, and 16.2 Å2 for
nitrogen), and has larger affinity forces (of attraction) due to its two-polar covalent bonds
(see Figure 60). Consequently, the water molecule can penetrate into more narrow spaces
(pores and texture) and will be more strongly adsorbed to the particles surfaces, relative to
the nitrogen molecule. A larger quantity of absorbed molecules, in a single layer, will
generate a larger BET-area. However, using water (moisture) is probably closer to real
conditions for materials for concrete production than using nitrogen gas.
H 2O + N2
H Adsorbed
molecules
+ N N
H O
-
Mono-layer
(~3.5Å for water)
Figure 60. The polar water (H2O)
molecule versus the non-polar
nitrogen (N2). Figure 61. Molecules adsorbed onto a surface
The technique of using the BET method with moisture (water) instead of nitrogen gas has
been applied by several researchers [4][156][127][159][162]-[165]. In the literature, it can
be seen that during the 1960s and early 1970s there was a vigorous debate on whether
water vapour should be used as BET-adsorbate. Traditionally, when using BET with water,
the focus has mainly been on internal porosity (e.g. to determine the pore size distribution
in a C-S-H gel) and not on external particle surface. Neither has the simplified method,
with different relative humidity instead of pressurized vapour, been used for particles.
Sample
Box with tight lid
Fan
Net
Figure 64. Photo of climate boxes with RH 11.3% (LiCl) and 33.1% (MgCl2) RH (left) and
their principle design (right).
The time for the samples to be conditioned and reach steady state within acceptance was
evaluated to be 3-5 days, depending on how large an area the material has. In Figure 65, it
is shown how the oven dried samples, exposed to 50% RH, increase in moisture content
with time. However, this is a relatively high RH.
0.5%
L10
L15
0.4%
Moisture content [%]
L25
0.3% L40
L180
0.2% L180X
L190
0.1%
MF
B15
0.0%
1 10 100 1000 10000
Time [hour]
Figure 65. Changes of moisture content with time, for seven limestone fillers: a glass filler
and a natural gravel (0-1 mm), conditioned at 50% RH. The time scale is logarithmic.
The repeatability was evaluated, using two different natural sands (1 and 2). Ten
repetitions were made, with double samples. New samples (2x100 g) were taken between
the runs. The results are presented in Figure 66. For each sample the coefficient of
variance (COV) was lower than 1.82%. A tendency can be observed, indicating that there
is a systematic error, yet not very large. There are numerous sources that can cause this
error, such as the conditioning time, weighing of oven-dried samples, measuring order, and
room temperature. No further investigation of this was made.
3600
1(average) 1a, COV 1.82%
2
3349 m /kg 1b, COV 1.55%
3500 1(average)
COV 1.65%
S(BETH2O)[m /kg]
3400
2
3300
Figure 66. Repeatability for the BET(H2O)-area, using double samples of two different
natural sands (0-0.5 mm). New samples (2x100 g) were taken between runs.
For gravel/aggregate, the removed particles not passing the 0.5 mm sieve can be
compensated for, but only very approximately. The BET(H2O) area (S´BETH2O) per unit
specimen mass is then calculated for the whole size fraction and approximated as:
m05
S ' BETH 2O = S BETH 2O ⋅ ( x05 + k ⋅ ( 1 − x05 )) [m /kg] [-]
2
(Eq. 37) x05 = (Eq. 38)
mtot
where k is a factor compensating for the removed particles not passing the 0.5 mm sieve,
x05 is the mass fraction passing the 0.5 mm sieve, m05 is the mass passing 0.5 mm, and mtot
is the total mass. If there is only a small amount passing the 0.5 mm sieve, the calculation
of S´BETH2O is not valid. In a series of measurements on four different 0-8 mm gravels
(naturals, sea sand and crushed), the area was measured on the fraction passing 0.5 mm as
well as on the whole fraction. The test was repeated three times, in order to ensure correct
measurements. The gravel’s size distribution is shown in Figure 67, and the measured
BET-area and factor is given in Table 8. For gravels with a maximum grain size up to 8
mm the factor was approximated to k ≈ 0.5.
100%
Table 8. Measures of BET(H2O)-area for the
80% fraction passing 0.5mm and the whole fraction,
Passing [%]
16
5
0
1
2
4
8
06
12
0.
0.
0.
0.
Size [mm]
Crushed 34% 4815 3102 0.46
Figure 67. Size distribution Average 0.51
In Paper II it was shown that the granular characteristics with the highest single correlation
was found between the BET(N2) and BET(H2O) measures (specific area). Although the
measured values are not equal, the linear relationship is good.
40 000
One has to be aware of the differences in
size and polarity of the water and nitrogen
S BET(H2O) [m /kg]
30 000
molecules. Tests have also been made on y = 1.554x
2
fines (<1.0 mm) sieved from different 20 000
2
R = 0.994
aggregates, with the same good
relationship. It was found that the 10 000
BET(H2O) was 1.55 times larger than
0
BET(N2), see Figure 68.
0 5 000 10 000 15 000 20 000
2
For binders of cement type, the BET(H2O) SBET(N2) [m /kg]
method did not supply reliable measures
Figure 68. The linear relation between
due to the nature of hydration, and is
measures of BET-area with N2 and H2O.
therefore not recommended.
The results from the flowability measurements in Papers II and III for mortars and
concretes show significant differences between the samples, which were strongly reflected
by the differences in BET(H2O)-area. There was a strong connection between the
BET(H2O)-area and the rheological parameters and slump flow values.
When there is a change in the dry material’s specific surface area, and as this area has to be
covered with water in order to create mobility, the concrete water demand will change.
One way to compensate for these variations in filler or fine aggregate, presented in Paper
III, is to consider the specific area by BET(H2O) and translate this to a change in water
demand of the concrete mix. With the assumption that 1 litre of water in one molecule
layer covers 3,546,000 m2, the change in mixing water (∆W) due to a change in specific
surface area (∆SBETH2O) can be calculated as:
nH 2O
∆W = ∆S BETH 20 ⋅ ⋅ m mtr [litre/m3] (Eq. 39)
3.546 ⋅ 10 6
where mmtr is the mass of the dry material of the mix, and nH2O is the number of full water
molecular layers covering the particle surfaces required to provide sufficient dispersion for
flowability. Based on numerous experiments, a suitable value was found to be nH2O ≈ 30
layers. This can be compared to the 5-20 molecular layers of water adsorbed at high
relative humidity, proposed in literature [4][156][127][159][166][167] or as much as 60
molecules in thickness [20]. Furthermore, it was shown that the free water content,
available to provide flowability, in 1 m3 SCC mix can vary by several litres due to
differences in apparently equivalent fine aggregates. In [5] it was found that a natural
gravel collected at different spots in a gravel pit, with small differences in grading, can
vary in BET(H2O)-area by ~7000 m2/kg. A change in BET-area of 1000 m2/kg corresponds
to approximately 0.8% moisture content of the gravel. E.g. a SCC with 1000 kg gravel (0-8
mm) that increases by 10000 m2/kg in area will need 8.5 litres of extra water, in order to
retain its consistency.
In Papers IV and IV the BET(H2O)-area was shown to influence – apart from the
flowability and water requirement – the pore pressure development, autogenous
deformation, plastic shrinkage and compressive strength. Limestone filler with larger BET-
area increased the rate and magnitude of autogenous shrinkage, primarily in the plastic
region, without affecting the temperature development and the times to initial and final set.
Increased particle surface area decreased the rate and magnitude of evaporation, and
reduced the plastic crack tendency. In addition, a larger BET-area gave rise to a higher
compressive strength. When adding extra water to the mix, compensating for the loss of
flowability due to increased particle surface area, the crack tendency increased
significantly, the autogenous shrinkage decreased and the compressive strength was
lowered.
For more details and a methodology description of the BET(H2O)-method, see Appendix A.
A strong correlation was found between the calculated specific area (from size
distributions) and the area measured with Blaine, whereas the correlation with the BET-
area was weak. This indicates that Blaine is mainly a measure of size and size distribution,
based on theoretical spherical particles. However, it should be noted that great variation
was observed between values measured on the same specimen, especially between those
performed by different persons (and equipment used).
Furthermore, the results presented in Paper II, shows that the effect of specific surface area
by Blaine for different filler materials showed a poor correlation with the mortar’s
rheological parameters.
The results, in Paper II, show that the correlations between the shape factors (F-shape, F-
circle and Compactness) are good. This was expected since the values used for calculation
have much in common. Thus it ought to be pointed out that F-shape is more a measure of
shape, F-circle is more a measure of texture, and Compactness is somewhere in between.
The correlation with other granular characteristics (calculated surface area, BET-area and
Blaine) was poor, and so was the connection with the mortar’s rheological parameters.
The quantification by image analysis can be problematic, as the method is strongly
dependent on a large number of factors, such as: sample preparation, microscope
performance, photo quality (sharpness), resolution, number of particles, analyzing
software, threshold technique, etc. Since the threshold was made manually, the results can
be somewhat arbitrary.
In Paper II, this method was used to quantify Mini-slump cone Sample
the different fillers’ retained water ratio (βp) ØD=700/100 mm Table (non-
H=60 mm adsorbent)
and deformation coefficient or sensitivity (Ep).
A mini-slump test was used to measure the Spread
flow spread. The relative flow area (Rp), at diameter
different water-to-powder ratios by volume
(Vw/Vp), was calculated as:
Figure 72. The mini-slump and the
D2 measurements of spread flow
R p = 2 − 1 [m2/m2] (Eq. 43)
D0 diameter (in four directions).
where D is the average spread diameter,
calculated in four directions and D0 is the base Vw/Vp [-]
diameter of the cone (see Figure 72).
The measure of retained water ratio (βp) can be Ep
considered as the amount of water, adsorbed on
the particle surfaces and filling the voids in the βp
particle system, needed to initiate flow. The Rp [-]
deformation coefficient (Ep) is a measure of the
sensitivity to a change in water content [169]. Figure 73. The evaluation of βp and
βp is represented by the interception point and Ep from the linear relationship of the
Ep the slope, from the linear relationship ratio of water to powder (Vw/Vp) and
between Vw/Vp and Rp (see Figure 73). relative spread flow (Rp).
Results, in Paper II, show a strong correlation between the fillers’ retained water ratio (βp)
and the mortar slump flow spread, whereas the deformation coefficient (Ep) correlated with
the specific surface area from size distribution and with the Blaine area. Theoretically, the
fillers’ retained water ratio (βp) should reflect the ability to adsorb water, and correlate
with the BET(H2O)-area; but this correlation was poor. In addition, the fillers’ water
absorption (with particles passing the 0.063 mm sieve removed) was determined in
according to EN 1097-6, a method mainly designed for aggregates. But as the coefficient
of variance was high (~25% when repeated four times) these measurements are not
presented. Still, the water absorption showed a correlation with the BET(H2O)-area.
4.4.2 Rheology
For a more scientific approach, a rheometer can be
used (see section 2.3). Unlike the measurements of
qualitative tests (e.g. slump flow), the rheological
parameters are fundamental physical quantities,
mutually independent and not dependent on
operator or equipment. The most established
parameters used to define mortar and concrete
rheology are the yield stress and plastic viscosity in
the Bingham equation [24][28] (see section 2.2.3) . Figure 76. The Bohlin CVO200.
For the mortars (in Papers I and II), a Bohlin
CVO200 rheometer was used, with a fixed outer
cylinder (cup) of diameter Do=30 mm and a
measuring rotating inner cylinder (bob) of diameter
Di = 20 mm, providing a gap of 5 mm (see Figure
76). For the concretes, (in Papers I, III and VI) a
ConTec Visco5 was used, with a rotating outer
cylinder of diameter Do=290 mm and a measuring
fixed inner cylinder of diameter Di=200 mm,
providing a gap of 45 mm (see Figure 77). Figure 77. The ConTec Visco5.
The two rheological parameters of plastic viscosity (ηpl) and yield stress (σ0) were
evaluated in accordance with the Bingham model, see (Eq. 7), at a controlled shear rate
( γ& ) at 20ºC. In addition, the experimental setup for mortars was initiated with a linear
up/down loop for a thixotropic evaluation, represented by the area in hysteresis (see Figure
14). The experimental geometry and measuring sequence is illustrated in Figure 78.
Thixotropy is not strictly a rheological definition, nor an absolute or fundamental term, but
a quantification of reversible time-dependence (see section 2.2.5). A typical measure of
mortar rheology is shown in Figure 79. The measure of segregation was used as a criterion
for acceptance (measures rejected when >10%).
60 No logging
Mortar sample
Logging
Shear rate [1/s]
45
H=37.5 mm
30
Rotating and
15 measuring
inner cylinder
0 Ri=10 mm Fixed outer
0 10 20 30 40 50 60 70 80 90 Ro=15 mm cylinder
Time [s]
8 No logging Ro=145 mm
Concrete
Logging Ri=100 mm sample
Shear rate [1/s]
4
H=140 mm
2 Measuring
inner cylinder
0 Rotating
0 10 20 30 40 50 60 outer cylinder
Time [s]
Figure 78. The measuring sequence for the Bingham evaluation (followed by segregation
estimation) and schematic illustration of the rheometers. For mortar the Bohlin CVO200
was used, and for concrete the ConTec Visco5. The sequence for mortars begins with a
linear up/down loop for a thixotropic evaluation.
1
Shear stress, σ [Pa]
2
Thixotropic area 3
Segregation [%]
Thixotropy [Pa/s]
Segregation
Viscosity, ηpl [Pa·s]
Figure 79. A typical measurement with mortar and the methodology evaluating the
Bingham parameters and thixotropy (and segregation).
0 001
0 001
Figure 81. Photo and illustration of the Concrete Digital Dilatometer (CDD), with
supplemented measurements of temperature and pore pressure.
For more details and a methodology description of the CDD-method, see Appendix B.
The result from a test is presented graphically and the development of deformation (mean
value from two or more tests) is plotted against time. Moreover, a number of deformation
factors were evaluated with a model presented in Figure 82. For concrete, the deformation
pattern comprises three distinct stages which can be defined as [91]: plastic, semiplastic
and rigid period. In the plastic (1) and semiplastic (2) periods, the rate of deformation
(dε/dt1 and dε/dt2), period time (t1 and t2) and deformation (ε1 and ε2) are evaluated from
the deformation/time graph. In the rigid period (3), the rate of deformation (dε/dt3) is
evaluated between 48 and 72 hours from water addition. The time (t) is related to the time
when the mixing water was added to the premixed solid material (including the cement).
As the measuring was started after 30 minutes, and as the initial deformation tends to be
linear up to 2 hours from mix, the curve was extrapolated to the time zero.
For the SCC mixes used in this work, the transition from plastic to semiplastic (t1) takes
place at ~6 hours after water addition and the transition to rigid period (t1 + t2) at ~12
hours. Compared to traditional concrete without addition of superplasticizer, the self-
compacting concrete (SCC) tends to be retarded for about one hour [91].
-6
ε1
dε/dt2 Final set
ε2
ε1+ε2 dε/dt3
t1 t1+t2
Time, t [hour]
2. Semi-
1. Plastic 3. Rigid
plastic
Figure 82. Model of how the deformation parameters are evaluated from the linear
autogenous deformation measurements, where the deformation is divided into
plastic/semiplastic/rigid periods.
It should be pointed out that linear measurement of autogenous deformation on a concrete
mix before setting, when the concrete is fresh, is a very sensitive task and must be made
with great care. A mean value from two or more tests, each with three complete CDD
setups, was used. A typical measurement (with three setups) generated a coefficient of
variance (COV) below 10% (see Figure 83). What can also be noted in Figure 83 is the
pattern of autogenous deformation, comprising the three distinct stages (plastic, semiplastic
and rigid), separated by the time to initial and final set, and manifested by a plateau in the
curve. Mortar, on the other hand, showed a different behaviour. In Figure 84, no
semiplastic region and distinct point of initial set could be observed, but merely a plastic
and a rigid period separated by a single point of set. Moreover, mortars generated more
stable measures with a smaller deviation (COV <5%), but then the magnitude of
deformation was also approximately two times that of the concretes.
It might seem that the development of autogenous shrinkage ends at final set, but it is
merely slowing down. In long-term measurements, following final set the autogenous
shrinkage after 9-12 months was approximately equal in magnitude as prior setting.
0 12% 0
Deformation [10 m/m]
COV -300
Deformation [10 m/m]
-200 8%
-6
-6
COV
-600
-400 Deformation 4%
(average) -900
-600 0% -1200
0 6 12 18 24 0 6 12 18 24
Time (from mix) [hour] Time (from mix) [hour]
For standard concrete (i.e. without additional filler and superplastisizer) a different
behaviour was also shown. In Figure 85 it can be seen that the initial shrinkage is
approximately half the shrinkage the SCC generates. And between initial and final set
(semiplastic region), the standard concrete generated much less shrinkage than the SCC.
These differences might be explained by the effects of the limestone filler and
superplasticizer. When limestone is added to a concrete, the initial induction period (or
dormant period) is shortened and an extra peak of hydration will occur [171]-[175]. This
phenomenon is explained by the surfaces of the filler material acting as nucleation sites for
the early reaction products of CH and CSH, which accelerates the hydration of cement
clinkers (especially C3S) [176]-[179]. In addition, if the cement has a significant amount of
tricalcium aluminate (C3A), calcium carboaluminate will be produced from the reaction
between calcium carbonate (CaCO3) from the limestone and the C3A [180]-[186], which
will also accelerate the hydration. On the other hand, the superplasticizer used for the
SCCs retarded the mixes by approximately one hour.
When developing the equipment, complementary tests were performed, evaluating the
effect of gravity on the measurements of autogenous deformation. Measurements with the
sample placed in 0 (horizontal), 30 and 60 degree positions show no significant differences
(see Figure 86), so the horizontal position was chosen for the method. However, to ensure
unrestrained conditions, a double layer of low-friction paper (teflon type or baking-tray
paper) was placed between the rig and the sample. In a series of tests, using a similar
dilatometer, and thus with a smaller tube, Mounanga et al. [150] evaluated the effect of the
mould’s position on the linear autogenous deformation on self-compacting mortars. It was
found that a vertical position generated more than three times the shrinkage that a
horizontal one did. This effect was mainly explained by sedimentation and bleeding of the
mortars.
-6
0° (horizontal)
30°
-400
60°
-600
0 6 12 18 24
Time (from mix) [hour]
Figure 86. The effect of gravity on the measurements, by placing the rig in different angles.
Steel rings
Climat
conditions:
23±2°C Concrete
35±5%RH specimen
PT100
Air velocity
Strain gauges
4.5 m/s
Pressure gauges
20 mm Steel ribs
80 mm
20 mm
ø300 mm Scale
ø600 mm
Figure 87. Illustration and photo, showing the test arrangement for the determination of
the cracking tendency.
The measurements start 60 minutes after mixing and the temperature, the weight loss and
the restraint strain are continuously recorded. After 20 hours of drying, the rings are taken
out of the rig and the cracking tendency is evaluated as the average total crack area (crack
length x crack width) on the concrete surface of each of the three specimens. The crack
width was measured with a crack microscope (to an accuracy of 0.05mm) and the crack
length was measured with a digital measuring wheel (to an accuracy of ±1mm). The
weight change was recorded, for one of three samples, using a scale (load cell based) with
accuracy better than 0.03% for a weight of 100 kg (minimum detectable weight change 20
g). The concrete temperature was measured using both a thermo thread, placed in the
specimen, and a PT100 sensor mounted on the inner ring. To monitor the stress build-up of
the concrete and the time when the cracks would appear, strain gauges were mounted (in
full bridge) on the inner steel ring. The air temperature and relative humidity in the room
were measured using a Visala sensor. In addition, the capillary pore pressure was measured
(at 20 and 60 mm depth). Plastic shrinkage is considered to be related to the capillary
pressure in fresh concrete [9][89][116]. The data (strain, pore pressures, weight,
temperatures and RH) were logged every minute using a data logger (PC-logger3100i from
INTAB).
For more details and a methodology description of the ring-test method, see Appendix C.
The method is intended for laboratory use and the test results are purely relative. They
cannot be directly transferred to predict the extent of cracking which will occur in practice
under the prevailing field conditions. Still, the underlying mechanisms can partly be
quantified in terms of temperature and pore pressure development. In order to verify the
ring-test method, Löfgren & Esping [192] conducted a field study in which the cracking
tendency was evaluated on the ring-test specimens, and on larger slab elements that were
both cast outside and exposed to the environment. A series of one reference and six
different SCC’s were used. The experimental results (see Figure 88) showed a strong
correlation (close to unity) between the ring-tests performed in the laboratory and the field
study (both the ring-test and the slab specimens).
3
Ring (field)
Relative crack area [-]
Slab (field)
2 Ring (lab)
0
Mix 1(ref) Mix 2 Mix 3 Mix 4 Mix 5 Mix 6 Mix 7
Figure 88. Comparison of the relative crack areas between the field study (the ring-tests
and the slabs) and the ring-tests of the laboratory study.
contracting negative capillary pressure will also develop, thus uniformly through the
member, but only once the hydration commences and the structure sets [89]. As long as the
concrete is plastic the capillary pore pressure undergoes only small changes. However, at
the stage where the concrete starts to set (initial set), and a restraining skeleton of hydration
products are formed, the capillary pore pressure reach an accelerating phase.
In Papers IV, V and VI, pore pressure was measured with pore pressure transducers (Model
AB 0-15 PSIG from Data Instruments 0-100 kPa / overload 200 kPa), connected to a de-
aired water filled system with a 50 mm long needle (cannula type) with an external/internal
diameter of 0.7/0.4 mm (see Figure 89). The test was performed according to a procedure
developed by Radocea [116]. The data were logged every minute using a data logger (PC-
logger3100i from INTAB). The measurements were performed on sealed samples (in
specimens for autogenous deformation), and on samples exposed to drying (ring-test).
De-aired water
filled system
Sample
Needle (cannula)
L 50 / Ø 0.4 mm
Pressure gauge
Figure 89. Picture and schematic illustration of pressure gauge and the needle used to
measure the capillary pore pressure in the concrete.
It should, however, be pointed out that this test technique is highly sensitive to local
conditions. This sensitivity manifests itself in, for example, a loss of pressure at a random
point in time. This point was named by Wittman [9] as the breakthrough pressure.
The breakthrough pressure probably occurs
0
with local disturbances at the needle tip, such
as destruction of the water menisci by air
Pore pressure [kPa]
5.1 Discussion
The distinguishing characteristic of self-compacting concrete (SCC) is its ability to flow
and consolidate under the influence of its own gravity weight. Yet it is a sensitive mix,
strongly dependent on the composition and the characteristics of its constituents.
Moreover, it has to possess the incompatible properties of high flowability together with
high segregation resistance – a balance made possible by the dispersing effect of high-
range water-reducing admixture (superplasticizer) combined with cohesiveness produced
by a high concentration of fines. However, the large specific surface area of the additional
filler material and the retarding effect of the superplasticizer will also promote the
autogenous (sealed) shrinkage and increase the risk of early-age cracking.
In this thesis, a literature review and experimental work were carried out in order to study
the rheology and early-age deformation of cementitious materials and factors affecting
them. The main conclusion from this work is that, due to the large surface areas involved,
quantification of geometrical and surface properties (size, shape, porosity and texture) of
fillers and the fine part of the aggregates is essential for the ability to control early-age
properties, such as workability and plastic shrinkage cracking, in the production of SCC.
In addition to the size and size distribution, the particles’ external characteristics were
found to be of major importance, especially their shape and texture. These characteristics
of three-dimensional bodies are rather difficult to describe, and it is therefore convenient to
use the total surface area as a single parameter. The surface area strongly reflects the water
requirement that is needed to create fluidity for the concrete. A commonly used method to
determine the specific surface area is the BET method, by which the area is deduced from
the amount of monolayer-adsorbed gas. The main difference between the BET method and
other traditional methods (e.g. that of Blaine) to determine the particles’ specific surface
area is that the BET provides more of a “real” surface area, as it includes shape and surface
properties, while most others are based on the assumption that all particles are spherical
and non-porous. For example, a coarser filler or gravel can provide a larger BET-area than
a finer one, due to differences in surface texture and accessible porosity. However, not
only the surfaces are to be covered with suspending media to generate fluidity; the voids in
between the particles are to be filled, and hence the particles’ packing will also have a
major influence on the flowability.
A simplified adsorption method, the BET(H2O) with water vapour as adsorbate, for
characterization of particles’ specific surface area was introduced, and is proposed as a
potential means of geometrical characterization for fillers and gravels. It is simple and low-
cost, and has provided stable and reliable values. It has also shown a strong correlation
with the traditional BET with nitrogen gas, as well as with the rheological properties.
Furthermore, it was shown that it is possible to calculate the extra water needed to
compensate for changes in filler and fine aggregates’ BET(H2O)-area, in order to produce
SCC with small variations in flowability. An increase in BET(H2O)-area of 1000 m2/kg
corresponds to a need for additional water of approximately 0.85% by mass of the gravel
(or filler) content for constant flowability. E.g. a SCC with 1000 kg gravel (0-8 mm) that
increases by 1000 m2/kg in area will need 8.5 litres of extra water, in order to retain its
swelling, approximately in the same magnitude after 24 hours as for the SCC’s with
cement. However, the SCC’s generated no swelling and almost all shrinkage before final
set (~12 hours), whereas for the mixes without cement the rate of shrinkage was lower in
this period. Moreover, once set the rate of deformation for the SCC’s significantly slowing
down. This indicates that not only the hydration (chemical shrinkage) is the driving
mechanism of autogenous shrinkage for concrete, but also the constituent’s
adsorption/absorption will contribute, especially in the fresh state before setting. For
cement paste, prior initial set, the chemical shrinkage might be equal to the autogenous
shrinkage. But once more or less porous particles (filler and aggregate) are introduced to
the mixture the adsorption/absorption will properly introduce an additional shrinkage.
o Increased particle surface area did not only decrease the SCC flowability, it also
decreased the rate and magnitude of evaporation and consequently reduced the
plastic crack tendency, despite an increased autogenous shrinkage. Moreover, an
increased area resulted in a higher compressive strength. However, with additional
water for constant flowability, compensating for the differences in BET(H2O)-area,
evaporation and plastic cracking tendency was increased significantly, and strength
was reduced.
o For concrete with a high w/c-ratio, evaporation was shown to be the main governing
mechanism for plastic shrinkage cracking, whereas for concrete with a low w/c-ratio
the autogenous shrinkage proved to be dominating. For mixes with retardation, both
the autogenous shrinkage and evaporation increased, and consequently so did the
crack tendency.
o It is proposed that not only the hydration (chemical shrinkage) is the driving
mechanism of autogenous shrinkage for concrete, but also the constituent’s
adsorption/absorption will contribute, especially in the fresh state before setting.
perhaps be to follow the sample’s weight as a function of time, frequently and long enough
to produce a smooth curve with a clear tendency, and extrapolate to an equilibrium state.
(2) Evaluate the effect of particles’ (filler, gravel and aggregate) adsorption/absorption
with time on the autogenous shrinkage of mortars and concretes. The hydration is, in
general, considered to be the single driving force of autogenous shrinkage. But the
measurements (in Paper IV) on mixtures without cement indicated a substantial
“autogenous” shrinkage, after an initial swelling. Consequently, the contribution of
adsorption/absorption to the autogenous shrinkage ought to be significant, especially in the
fresh state, before initial setting. More measurements need to be made, using different
compositions and materials, and to be complemented with pore pressure measurements on
mixtures without cement.
(3) Develop methodology for measuring the plastic shrinkage, using the concrete
dilatometer (CDD) with an open system where the samples are exposed to evaporation. If
the measurements are made simultaneously with the sealed system, the evaporation
shrinkage can be extracted from the plastic shrinkage. Yet the plastic shrinkage will only
be relative, and so will the evaporation shrinkage, as these measures will depend on the
geometry and diffusion coefficient of the mould, exposed area, air velocity, RH,
temperature, etc.
Within this work, an attempt was made
to measure the plastic shrinkage with (b)
the CDD, by replacing the PE-tube with
a felted cloth (geotextile/fabric; see
Figure 91). But as this mould did not
have the radial stiffness (e.g. from
corrugation and steel wire coil), the (a)
shrinkage in the plastic stage was
mainly transformed to vertical
displacements and almost no linear
measurements were recorded in this
stage. Hence, the open (diffusion)
mould needs to be designed with a Figure 91. Measurements with the CDD: (a)
relation between the volumetric, radial under sealed conditions, and (b) when
and longitudinal deformations, equal to exposed to evaporation (plastic shrinkage).
the sealed mould.
In the present study, the fundamental mechanisms affecting the rheology of cementitious
materials were theoretically reviewed. However, to be able to practically use and apply
these theories in “reality”, a large experimental study needs to be made and the results
compared with those in the literature. The study should focus on the mix design of high-
flowable concretes (e.g. SCC), in which the proportions of the constituents and their
properties are of major importance. Recommendations or instructions for how the
proportions and properties affect the workability/rheology of concrete should be given, e.g.
by designing a flow diagram with orientation (see Figure 92). Also how different measures
of the constituents, by specific methods, affect the workability/rheology are to be given. To
be able to ensure the quality and hopefully lower the cost in the production of SCC, such a
guideline could be a helpful tool.
FLOW DIAGRAM
+Irregularity
Yield stress, σ0 [Pa]
+Elongation
+Air
+Paste volume
Figure 92. Illustration of a flow diagram, showing how changes in proportions and
properties of constituents may affect the flow behaviour (rheologically in terms of the
Bingham parameters σ0 and ηpl) of fresh concrete. This is a potential aid in mix design,
showing how to best orientate towards a desired point of consistency.
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Annual Book of ASTM Standards, Volume 04.02, 2002.
ASTM C204-00, “Standard test method for fineness of hydraulic cement by air permeability
apparatus”, 2002.
ASTM C403, “Test method for time of setting of concrete mixtures by penetration resistance,
Annual Book of ASTM Standards, Vol. 04.02, 2002.
ASTM C426-06 Standard test method for linear drying shrinkage of concrete masonry units,
Annual Book of ASTM Standards, Vol. 04.05, 2006.
ASTM C1608-06, “Standard Test Method for Chemical Shrinkage of Hydraulic Cement Paste”,
Annual Book of ASTM Standards, Vol. 04.01, 2006.
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EN 196-3, “Methods of testing cement - Part 3: Determination of setting time and soundness”,
2005.
EN 933-1, “Tests for geometrical properties of aggregates - Part 1: Determination of particle size
distribution - Sieving method”, 2004.
EN 933-2, “Tests for geometrical properties of aggregates - Part 2: Determination of particle size
distribution - Test sieves, nominal size of apertures”, 1996.
EN 1015-2, “Bulk sampling of mortars and preparation of test mortars - Part 2: Bulk sampling of
mortars and preparation of test mortars”, 2006.
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mortar (by flow table)”, 1999.
EN 1097-6, “Tests for mechanical and physical properties of aggregates - Part 6: Determination of
particle density and water absorption”, 2000.
EN 12350-2, “Testing fresh concrete - Part 2: Slump test”, 2000.
ISO 2884, “Paints and varnishes: Determination of viscosity using rotary viscometers - Cone-and-
plate viscometer operated at a high rate of shear”, 1999.
ISO 3219, “Plastics; Polymers/resins in the liquid state or as emulsions or dispersions -
Determination of viscosity using a rotational viscometer with defined shear rate”, 1993.
ISO 9277, “Determination of specific surface area of solids by gas adsorption using BET method”,
1996.
NT BUILD 433, “Concrete: Cracking tendency – Exposure to drying the first 24 hours”, Nordtest,
1995.
NT BUILD 486, “Aggregates: Size distribution”, Nordtest, 1998.
RILEM report 25, “Early Age Cracking in Cementitious Systems, TC181-EAS, RILEM Technical
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SS 132126, “Concrete testing - Aggregate - Modulus of fineness”, 1986.
SS 134222, “Methods of testing cement - Determination of fineness”, 1990.
APPENDIX A: BET(H2O)
DETERMINATION OF SPECIFIC SURFACE AREA OF FILLER AND FINE
PART OF AGGREGATE BY BET METHOD WITH WATER ADSORPTION.
BET(H2O):
DETERMINATION OF SPECIFIC SURFACE AREA OF FILLER AND FINE
PART OF AGGREGATE BY BET METHOD WITH WATER ADSORPTION
Key words: surface area, BET, adsorption, powder, filler, aggregate.
1 SCOPE 3 REFERENCES
This description provides guidelines for [1] Brunauer S., Emmet H. P., Teller., “Adsorption
determination of specific surface area by the of gases in multimolecular layers”, American
BET(H2O) method. The principle is based on the Chemical Society, 1938.
method of Brunauer, Emmet and Teller [1], where
[2] Gregg S. J., Sing K. S. W., “Adsorption, surface
the area is given by the number of physically
area and porosity”, New York, 1967.
adsorbed gas molecules formed in a monolayer.
For a general description of the BET method see Standard: ISO 9277, “Determination of the specific
ISO 9277, and for the physics and applications of surface area of solids by gas adsorption using the
gas adsorption see Gregg and Sing [2]. The BET method”, 2002.
measurements of BET area are normally
conducted volumetrically with nitrogen gas (N2), but Standard: EN 933-1, “Tests for geometrical
in this case it is gravimetrically with water vapour properties of aggregates - Determination of particle
size distribution - Sieving method”, 2004.
(H2O) as adsorptive gas. By using the relationship
between the relative humidity and the adsorbed Standard: EN 1097-5, “Tests for mechanical and
weight per unit specimen mass the surface area is physical properties of aggregates - Determination
calculated (in m² per kg). The BET(H2O)-area is of the water content by drying in a ventilated oven”,
generally much larger than the area determined by 2004.
air permeability (e.g. Blaine), and slightly larger
than the BET(N2)-area due to the differences in Standard: EN 932-1, “Tests for general properties
polarity and molecular size. of aggregates - Methods for sampling”, 1997.
For concrete, particle concentration and size Standard: EN 932-2, “Tests for general properties
distribution strongly influence the workability since of aggregates - Methods for reducing laboratory
its matrix consists of a suspension of smaller samples”, 2004.
particles filling the hollow spaces between the
coarser ones. To decrease the internal friction and
generate mobility, the particle surfaces are to be 4 NOTATIONS
covered with water and the voids in the system to 4.1 Definitions
be filled. Other important properties affecting the
workability are the particle shape, porosity and Adsorbate; A substance that is adsorbed at the
surface texture. Since surface area/volume ratio interface of a substrate material.
increases exponentially with particle irregularity Adsorbent; The substrate material onto which a
(shape, surface texture and porosity) and substance is adsorbed.
decreased size, quantification of geometrical
properties of fillers and the fine part of the Adsorption; Enrichment of adsorptive at the
aggregates is essential for the ability to control external and accessible internal surfaces of a solid.
physical properties, such as workability.
Adsorptive; A measuring gas to be adsorbed.
Adsorption isotherm; A graphical representation of
2 FIELD OF APPLICATION the relationship between the bulk activity of
adsorbate and the amount of adsorbate at constant
The BET(H2O) test method is only to be applied for temperature.
laboratory use on fillers and fine part of aggregates.
Cement and other powders reacting with water are BET; A model to determine the surface area from
not to be analyzed. Maximum particle size is 0.5 the physical adsorption of a gas on a solid surface,
mm. If the material incorporates particles up to 8 named after Brunauer, Emmett & Teller.
mm, these are to be removed and compensated Specific surface area; The ratio of total (external
for. For materials with particles larger than 8 mm, and corresponding internal) surface area per unit
the BET(H2O) method is not recommended. weight or unit volume.
NOTE 2: Two containers for each material are h) Weigh the sample and determine the mass
needed as the sample is to be made in pairs, to (m2) by subtracting the mass of the tray (mc) from
ensure precision. the measured weight.
b) If the materials contain grains larger than 0.5 NOTE 6: Keep the lids of the boxes as closed as
mm these are to be removed by sieving. The possible between the weighing of samples. The
masses of the passed and retained materials on saturated salt solution can be reused a large
the 0.5 mm sieve (see EN 933-1) are to be number of times. Just ensure that the salt is
weighed and recorded. sufficiently moistened, but not fully dissolved.
Adjust by adding extra salt or water if needed.
c) The ~100 g specimens (two per material) are
to be placed in each container. NOTE 7: It is also possible to determine the dry
mass of the test portion (see d to f) as a final step
d) The samples and the desiccant are to be instead. For higher precision and lower error, the
placed in the ventilated drying oven with a dry mass can be determined both initially and
temperature of 110±5°C. The time to dry depends finally (and the mean value reported). The dry
on the sample’s size, fineness, porosity and mass should not differ by more than 0.01%.
moisture content. A minimum time of 4 hours is
recommended. 5.4.2 Finishing the test
e) The samples and the desiccant are to be The measured masses (mdry, m1, and m2) for each
placed in the desiccator or airtight cabinet. The test portion are to be transferred to a computer for
time required for the cooling stage depends on the calculation and evaluation.
size and number of samples, the tightness of the
cabinet, balance heat sensitivity, etc. Time less
than 2 hours is recommended. 5.5 Expression of results
NOTE 3: It is also possible to weigh a sample The BET(H2O) surface area per unit specimen
immediately after removing it from the oven if the mass is calculated as:
balance is sufficiently protected from the sample
heat (with e.g. a cork mat). 3.54 ⋅ 10 6
S BETH 2 O = [m2/kg] (Eq. 1)
f) Weigh the samples and determine the dry a+b
mass of the specimen (mdry) by subtracting the where a is the interception point and b the slope of
mass of the tray (mc) from the weight. Directly place the curve from the linear relationship between the
the sample in the climate box with 11.3% RH (LiCl). BET(H2O) adsorption isotherm and relative
The time for the test portion to be conditioned is a humidity (see Figure 1b). The adsorption isotherm
minimum of 3 days, preferably 4-5. The box is to be (y) is calculated as:
placed in a thermally controlled room or chamber
with an air temperature of 20±2ºC. RH
y= [kg/kg] (Eq. 2)
NOTE 4: The time when the sample is exposed is
u ⋅ ( 1 − RH )
crucial, and is to be kept as short as possible. where RH is the relative humidity (0.113 and
NOTE 5: In some cases where the particles are 0.331), and u is the moisture content of the
very fine (e.g. silica fume) or very porous, a longer conditioned specimen. The moisture content is
time is needed for conditioning. The time required calculated as:
to achieve constant mass for a specific type of
(m − mdry )
material, or particle size, can be determined by u= [kg/kg] (Eq. 3)
successive weighing at least 12 h apart and seeing mdry
that the mass does not differ by more than 0.005%.
where mdry is the mass of the oven-dry specimen
and m the mass of the conditioned specimen (m=m1
for 11.3% and m=m2 for 33.1%).
y [kg/kg]
b
Fan
a
Net
0.113 RH [-] 0.331
(a) (b)
Figure 1. (a) Schematic illustration of climate box, and (b) the BET-plot with adsorption isotherm as a linear
function of RH.
1 SCOPE 4 NOTATIONS
This test method covers determination of concrete 4.1 Definitions
autogenous deformation. It has the ability to start
measurements before setting, when the concrete is Linear deformation; the relative change in length
fresh. The method is a modification of the CT1 due to shrinkage or expansion, referred to the
digital dilatometer for pastes and mortars. specimen’s original length.
As the use of high-performance and self- Autogenous deformation; the unrestrained, time-
compacting concrete has increased, problems with dependent bulk deformation of fresh and hardening
early-age shrinkage and cracking have become sealed concrete at a constant temperature.
significant. Conditions such as reduced water- Shrinkage; when the deformation is a contraction, it
cement ratio, reduced maximum aggregate size, may be referred to as shrinkage, e.g. autogenous
increased amount of fines, and increased binder shrinkage.
content all contribute to these problems. Compared
with drying shrinkage, which generally occurs from Chemical shrinkage; under sealed conditions, the
the outer surface of the concrete inward, cement paste hydration products occupy less
autogenous shrinkage develops uniformly through space than the original reactants. Most factors
the concrete member, but can be more likely to causing the autogenous shrinkage are chemical.
cause cracking, because it develops more rapidly
and occurs when the cement paste is young and
has poorly developed mechanical properties. 4.1 Symbols
With the concrete digital dilatometer test, the fresh ∆l change in length of specimen at time t, in
and hardening concrete linear autogenous micrometres [µm].
deformation is evaluated. t time after mixing (when measurements
The test is only to be applied for laboratory use. start), in hours and minutes [hh:mm].
Maximum coarse aggregate size is 16 mm. ε relative change in length, defined positive
for shrinkage (negative for swelling), in
A concrete digital dilatometer (CDD) test is microstrain [µm/m].
preferably combined with:
T concrete cross section temperature, in
• Cracking tendency ring-test (NT BUILD 433) for degrese Celsius [ºC]
concrete.
0 001
0 001
Figure 1. Principe of the Concrete Digital Dilatometer (CDD) for autogenous measurement.
1 SCOPE 3 REFERENCES
This test method covers determination of concrete Sampling procedure: EN 12350-1, ASTM C172 or
cracking tendency at early ages. The test is NT BUILD 191.
performed on 3 restrained ring-shaped specimens,
Cracking tendency test: NT BUILD 433
exposed to an air stream of defined velocity,
temperature and relative humidity, for the first 24
hours after casting.
4 NOTATIONS
The principle of the test is that the concrete sample
is cast around a restraining inner steel ring, causing 4.1 Definitions
a development of tangential stresses, which if Shrinkage: when the deformation is a contraction, it
sufficiently high may lead to cracking. The may be referred to as shrinkage, e.g. autogenous or
evaluation is based on characterization of the cracks drying shrinkage.
in terms of average total area in the three samples.
Autogenous shrinkage: the unrestrained, time-
The method is a modification of the Nordtest method dependent bulk deformation of fresh and hardening
“NT BUILD433”. sealed concrete at a constant temperature.
Problems with early-age shrinkage and cracking Chemical shrinkage: under sealed conditions, the
have become significant. Conditions such as cement paste hydration products occupy less space
reduced maximum aggregate size, increased than the original reactants. Most of the factors
amount of fines, presence of retarding admixtures, causing the autogenous shrinkage are chemical.
increased binder content and deficient covering and
curing all contribute to these problems. Evaporation shrinkage: when water evaporates from
the fresh and hardening concrete, tensile stress
Most probably the plastic shrinkage also consists of builds up in the capillaries, causing the concrete to
autogenous shrinkage. Compared with autogenous contract. In early stages; drying shrinkage can be
shrinkage, which generally develops uniformly defined as plastic shrinkage.
through the concrete member, shrinkage due to
evaporating occurs from the outer surface of the
concrete inward, causing cracks that develop 4.1 Symbols
rapidly, and occurs when the cement paste is young
and has poorly developed mechanical properties.
n number of cracks of each specimen.
l length of each crack, in millimetres [mm].
2 FIELD OF APPLICATION w each crack average width, in millimetres
With the “Concrete cracking ring test”, the plastic [mm].
and hardening concrete cracking tendency can be A average total crack area calculated from two
used for an evaluation of different types of concrete ore more samples, in sq. millimetres [mm2]
exposed to early drying.
t time after mixing, in hours [h].
The test is only to be applied for laboratory use,
where the method information is relative and cannot ∆m sample weight loss due to drying, in
predict the extent of cracking which might occur kilograms [kg].
under prevailing conditions. E sample evaporation, in kilograms per sq.
Maximum coarse aggregate size is 16 mm. metre [kg/m2].
The concrete cracking ring test is preferably v air velocity, in metres per second [m/s].
combined with: RH air relative humidity, in percentage [%].
• Volume or linear measurement of autogenous Ta air temperature, degrees Celsius [ºC].
deformation, e.g. Concrete Digital Dilatometer
(CDD) test for concrete. Tc concrete temperature, degrees Celsius [ºC].
The recording phase (t, Tc, ∆m, Ta and RH) stops. e) Purpose of test.
Values are to be transferred to computer for f) Concrete ID (producer, recipe, etc).
calculation and evaluation.
g) Identification of the test equipment and
instruments used.
5.4.3 Crack measurements h) Method of sampling.
The ring specimens should normally be examined i) Time from water addition to sampling start/stop
after 24 hours’ exposure, and surface cracks with an and crack measuring.
approximate radial orientation should be identified
j) Air velocity (v), temperature (ta) and humidity
and marked in an adequate way. The average width
(RH) during the test.
(w) and length (l) of each crack are to be measured
and recorded. The width measurements shall be k) Test results: number of cracks (n), total crack
performed by the use of the magnifying glass and area (A) and graphical presentation of concrete
readings by interpolation to the nearest 0.02 mm. It temperature and evaporation (t, Tc and E).
is recommended that a lower crack limit is 0.05 mm.
The main crack pattern of each ring can be recorded l) Relevant visual observations and personal
by photo or sketched by drawing. judgments and interpretations.
The standard procedure also includes recording of m) Any deviation from the test method.
weight loss and temperature development. These n) Inaccuracy and/or uncertainty of test results.
parameters give useful information about the
evaporation of water, and serve as a control for o) Date and signature.
identical tests as well.
Fan
Adjustable damper
Duct ø100 mm
Distances 10 mm
Test arrangement
30°
120°
Distances
h=10 mm
Transparent, e.g.
Plexiglass, t=4 mm Steel ribs 80 x 25 x 3 mm,
25
12 pcs on outer & 3 pcs on inner ring
11°
51
80
ø100
6
ø612
ø300 (outer)
ø600 (inner) 6
Figure 1. Principe of the concrete cracking ring test for cracking tendency measurement.
APPENDIX D: GLOSSARY
The following terminology, related to the subject matter in this work, has been adopted.
Thus some modification from its origins is made (see references at end of this appendix).
This glossary is intended as a reader’s aid. The explanations given here are not rigorous
definitions and should not be regarded as such. Formal definitions may be found in
documents such as:
o ASTM Standard C125 “Standard terminology relating to concrete and concrete
aggregates”
o British Standard BS5168 “Glossary of rheological terms”
o ACI Manual 116R “Cement and concrete terminology”
o European standard EN 197-1 “Cement”, EN 206-1 “Concrete”, EN 934-2
“Admixtures for concrete”, EN 12620 “Aggregates for concrete”
Definitions regarding fresh concrete and mortar and its constituents are fairly well defined
in literature and standards. However, an established and standardized terminology is
somewhat more deficient regarding the subject of early-age deformation, and especially
autogenous deformation.
admixture: A material other than water, aggregates, and cement, that is used as an ingredient of
concrete and is added to the bath before and during the mixing operation.
adsorbate: A substance that is adsorbed at the interface of a substrate material.
adsorbent: The substrate material onto which a substance is adsorbed.
adsorption hysteresis: The adsorption and desorption curves’ deviation from one another. Generally
explained as due to the ink-bottle effect.
adsorption isotherm: A graphical representation of the relationship between the bulk activity of
adsorbate and the amount of adsorbate at constant temperature.
adsorption: Development at the surface of a solid of a higher concentration of a substance than what
exists in the bulk of the medium. For aggregate, concrete and cement, adsorption is the formation of a
layer of water at the surface of a solid held by either physical and/or chemical forces.
aerosol: Droplets or particles dispersed in a gaseous phase.
aggregate: Granular material, such as sand, gravel, crushed stone, or crushed concrete, used with a
hydraulic cementing medium to produce either concrete or mortar.
aggregation: A general term defined as any process by which particles collect to form a cohesive mass
or cluster structure.
anti-thixotropy: See negative thixotropy.
apparent density: The density of loose or compacted particulate matter determined by dividing actual
weight by volume occupied; apparent density is always less than true density of a material comprising
the particulate matter, because volume occupied includes the space devoted to pores or cavities between
particles (see apparent particle volume).
apparent particle volume: The total volume of the particle excluding open pores, but including closed
pores.
apparent viscosity, The quotient of shear stress divided by shear rate when the this quotient is
filler: A general term for very fine granular material of solid material, usually inert and less than
roughly 0.125 mm, which occupies space and may improve physical properties or lower costs. Filler
can either be an additive or a fine fraction of aggregate (see powder).
filling ability: The concrete's ability to flow into and fill the mould.
final setting: Structural phase of the cementitious system matrix transforming to a true rigid, controlled
by its hydration. The final setting is manifested by an increasing strain capacity and a distinct decreased
rate of autogenous deformation. At the transitional period between initial and final set, the matrix
changes from true fluidity to true rigidity state.
fine aggregate: A general term for aggregate of such size that it substantially passes a sieve of specified
size, commonly 8.0, 4.0 or 4.75 mm.
fineness modulus: An index of fineness or coarseness of an aggregate sample. An empirical factor
determined by adding total percentages of an aggregate sample retained on each of a specified series of
sieves, and dividing the sum by 100.
fines: Material in aggregate finer than a given sieve, usually the 0.125 or 0.074 mm sieve (see powder).
Used for expressing the amount of fine aggregate in a concrete mixture as a percent by absolute volume
of the total amount of aggregate.
flocculation: The process by which particles in a suspension are mutually attracted by a combination of
van der Waals and electrostatic forces, stick together to form agglomerates and either settle out of the
suspension as flocs or form a three-dimensional network throughout the suspension.
flow curve: A graphical representation of the material's flow behaviour in which shear stress is related
to shear rate. The flow curve is a type of rheogram.
flow hysteresis: A condition resulting from differences in the rate of energy dissipation due to shear
history. In a typical rheometric test, shear stress or shear rate is ramped at a fixed speed up to a
maximum value, and then ramped back down at the same speed to the beginning. In hysteresis, one
flow curve lies above the other, forming a continuous loop whose internal area depends on the shear
and thermal history of the material, and on how rapidly the stress or shear rate was ramped. If the
down-curve lies below the up-curve, then it is referred to as a thixotropic loop, whereas if the down-
curve lies above the up-curve, then it is called a negative thixotropic loop. The area enclosed in this
loop is a commonly used measure of thixotropy/anti-thixotropy.
flow: Time dependent irrecoverable deformation.
flowability: A measure of the consistency of freshly mixed concrete, mortar, or cement paste. Usually
expressed in terms of spread diameter of a slump flow test (see workability).
fluidity: The reciprocal of viscosity.
free moisture: Moisture having essentially the properties of pure water in bulk; moisture not absorbed
by aggregate. See also surface moisture.
F-shape: A shape measure, calculated as the ratio of the length of the minor axis to the length of the
major axis. If the elongation is 1, the object is roughly circular or square.
grading: See size distribution.
grout: A mixture of cementitious material and water, with or without aggregate, proportioned to
produce a pourable consistency without segregation of the constituents; also, a mixture of other
composition but of similar consistency.
Herschel-Bulkley: A three-parameter rheological model used to describe viscoplastic materials
exhibiting a yield response with a shear-thinning relationship above the yield stress.
hydration: Chemical reaction which takes place as a result of combining cement and water. Maximum
hydration equals maximum potential strength of cementitious materials.
initial setting: Transition phase of cementitious system when the matrix changes from a concentrated
suspension of flocculated particles to a viscoelastic skeletal solid capable of supporting an applied
stress. At initial setting, capillary pore pressure rises significantly. Before initial setting, the chemical
shrinkage is equal to the autogenous shrinkage, and furthermore, the total shrinkage will transform into
settlement.
linear deformation: The relative change in length due to shrinkage or expansion, referred to the
specimen origin length.
liquid phase: Consisting of a condensed fluid, e.g. the dispersion or suspending media in a suspension.
mixing water: The water in freshly mixed sand-cement grout, mortar, or concrete, exclusive of any
previously absorbed by the aggregate (e.g., water considered in the computation of the net water-cement
ratio). See also surface moisture.
mobility: An ability of a fresh mix to flow and fill formwork or other container spaces.
moisture content of aggregate: The ratio, expressed as a percentage, of the weight of water in a given
granular mass to the dry weight of the mass.
monolayer adsorption: Adsorption in which only a single layer of molecules becomes adsorbed at an
interface. In monolayer adsorption, all adsorbed molecules are in the position of closest approach to the
substrate surface.
mortar: Concrete with essentially no aggregate larger than about 4 mm, i.e. a mixture of cement, sand
and water.
negative thixotropy: A reversible time-dependent increase in viscosity at a particular shear rate.
Shearing causes a gradual growth in structure over time (see flow hysteresis).
Newtonian: A flow model of fluids in which a linear relationship exists between shear stress and shear
rate, where the coefficient of viscosity is constant with shear rate ( σ = γ& ⋅ η ).
particle phase (or solid phase): The particles in a suspension, gel or aerosol.
particle size distribution: The division of particles of a graded material among various sizes; for
concrete materials, usually expressed in terms of cumulative percentages larger or smaller than each of
a series of diameters or the percentages within certain ranges of diameter, as determined by sieving.
particle: Any condensed-phase three-dimensional discontinuity in a dispersed system may generally be
considered a particle. The term is normally used in reference to solid materials. An aggregate may also
be regarded as a particle.
passing ability: The concrete's ability to flow through narrow spaces and prevent blocking around
reinforcements.
paste: The fraction of concrete comprising powder (including cement), water, air and admixtures.
plastic shrinkage: Net sum of early-age volume changes, including autogenous shrinkage and
shrinkage due to loss of water caused by evaporation, the aggregates' and filler materials' adsorption and
absorption, and suction of water by sub-base or formwork material.
plastic viscosity: The excess of shear stress over yield stress divided by the shear rate (see Bingham
model). In a flow curve, the viscosity is represented as the slope of the curve. For concrete, mortar or
other non-Newtonian materials, the term is often used synonymously with viscosity.
plastic: The property of a solid body that is in the elastic state when the stress is below a critical value,
termed the yield stress, and in plastic state when this value is exceeded.
plasticizer: An admixture which increases workability/flowability of freshly mixed mortar or concrete
without increasing water content. Also known as water-reducing admixture because it can maintain the
same workability/flowability of the mix with reduced water content.
plug flow: Flow in a pipe of a material that possesses a yield value (see yield stress). Because of the
existence of the yield value, flow starts near the surface of the pipe and the material flows forward as a
solid plug (i.e. the core of the material has a zero velocity gradient).
porosity: The ratio, usually expressed as a percentage, of the volume of voids in a material to the total
volume of the material, including voids.
Portland cement: A finely pulverized clinker produced by burning mixtures containing lime, iron,
alumina, and silica at high temperature and in definite proportions, and then intergrinding gypsum to
give the properties desired.
powder: A general term for relatively dry, undispersed accumulation of very fine granular material of
solid material including cement and those having a fineness equal to cement. Maximum dimension in
any given direction is less than roughly 0.125 or 0.074 mm. It will also include this size fraction of
aggregate.
precision: The degree of agreement within a set of observations or test results obtained as directed in a
test method.
pseudoplastic: See shear thinning.
relative humidity: The ratio of the quantity of water vapour actually present to the amount present in a
saturated atmosphere at a given temperature; expressed as a percentage.
relaxation time: A time characterizing the response of a viscoelastic material to the instantaneous
application of a constant strain.
repeatability: Variability of independent test results obtained on the same material, with the same
equipment, and by the same operator.
reproducibility: Variability of the replicated results of same test method, obtained on identical material
performed by different operators using different equipment.
retained water ratio: The amount of water, adsorbed on the particle surfaces and filling the voids in
the particle system, needed to initiate flow.
retardation time: A time characterizing the response of a viscoelastic material to the instantaneous
application of a constant stress.
rheology: The science of the deformation and flow of matter.
rheometer: An apparatus for measurement of rheological properties.
rheopexy: An effect by which a material recovers some of its pre-sheared viscosity at a faster rate when
it is gently sheared compared to when it is allowed to stand. The term 'rheopexy' is commonly used in
practice to indicate negative thixotropy, although this usage is strictly incorrect.
robustness: The concrete's ability to resist deviation in the constituents' proportions (water, cement,
aggregate and additives) and properties (gravel moisture content, aggregate grading, etc.).
roundness: The ratio of the average radius of curvature of the several edges of corners of a particle to
the radius of curvature of the maximum inscribed sphere.
sand: The fine granular material (usually passing the 4 mm sieve and predominantly retained on the
0.125 mm) resulting from the natural disintegration of rock, or from the crushing of friable sandstone.
saturation: The condition of coexistence in stable equilibrium of either a vapour and a liquid or a
vapour and solid phase of the same substance at the same temperature. Applied to aggregate or
concrete, the condition such that no more liquid can be held or placed within it.
segregation: A loss of uniformity of fresh concrete mix. A separation of one or more of the constituents
of the mix with consequent non-uniform proportions.
self-compacting concrete: A modified standard concrete that, without the influence of additional
compaction energy, flows, de-airs and completely fills the formwork only under the influence of its
own gravity weight. It has to combine high fluidity with a high segregation resistance and has to be able
to carry coarse aggregate grains through narrow spaces.
self-desiccation: Lowering of internal relative humidity in a closed isothermal cement paste system due
to the consumption of capillary water and the chemical shrinkage from progress of cement hydration.
separation: The tendency, as concrete is caused to pass from the unconfined ends of chutes or
conveyor belts, for coarse aggregate to separate from the concrete and accumulate at one side; the
tendency, as processed aggregate leaves the ends of conveyor belts, chutes, or similar devices with
confining sides, for the larger aggregate to separate from the mass and accumulate at one side; the
tendency for solids to separate from the water by gravitational settlement. See also bleeding and
segregation.
setting: Onset of solidification in a plastic cement paste system. The beginning of solidification,
referred to as initial set, marks the point in time when the paste loses its plasticity, becomes unworkable
hardened concrete.
surface voids: Cavities visible on the surface of a solid. See also porosity and surface texture.
suspension: A liquid in which solid particles are dispersed (see dispersion).
thixotropy: A reversible time-dependent decrease in viscosity at a particular shear rate. Shearing causes
a gradual breakdown in structure over time. The thixotropy is a measure of applied work needed to
break down the structure. In a flow curve, the thixotropy causes a flow hysteresis effect (see flow
hysteresis). Note that thixotropy is a reversible phenomenon; the term is often used wrongly in concrete
technology to describe an irreversible change.
van der Waals force: A short-range electromagnetic force interacting between two non-polar
molecules (or atoms), where the force arises when the molecules become polar for a short time because
their electrons are in constant motion. This motion is usually balanced or symmetrical around the non-
polar molecule, but if the electrons are briefly disturbed their negative charge may increase at one part
of the molecule, creating a positive charge on another part of the molecule. The molecule becomes a
dipole for a short time until the electrons rebalance, disturbing electrons in neighbouring molecules,
turning them into dipoles as well. The force also acts between macroscopic bodies, as particle-particle
and particle-surface, where if two solid surfaces are brought close together, all the atoms in the surface
zones will contribute to the forces of attraction. The van der Waals forces are much weaker than the
force that arises from electrostatic charged particles, but are strong enough to hold some particles
together.
vapour pressure: The pressure exerted by a vapour that is calculated from relative humidity and
temperature. The higher the humidity, and the higher the temperature in degrees Celsius, the greater the
vapour pressure exerted.
viscoelastic: A time-dependent property in which a material under stress produces both a viscous and
an elastic response. A viscoelastic material will exhibit viscous flow under constant stress, but a portion
of mechanical energy is conserved and recovered after stress is released.
viscoplastic: A hybrid property in which a material behaves like a solid below some critical stress
value, the yield stress, but flows like a viscous liquid when this stress is exceeded. Often associated
with aggregated particle suspensions (e.g. mortar and concrete).
viscosity: The property of a Newtonian material to resist increased deformation increasingly with
increasing rate of deformation. It is determined as the ratio of shear stress to shear rate ( η = σ / γ& ) in a
steady flow. For concrete or other non-Newtonian materials, often used synonymously with plastic
viscosity (or apparent viscosity).
viscous: The tendency of a liquid to resist flow as a result of internal friction.
water-cement ratio: The ratio of the amount of water, excluding only that absorbed by the aggregates,
to the amount of Portland cement in a concrete or mortar mixture; preferably stated as a decimal by
weight.
workability loss: The amount by which the workability of freshly mixed concrete changes during a
period of time after the initial mixing. Traditionally expressed in terms of the decrease in spread
diameter of a flow cone test.
workability: A general term relating to behaviour of fresh concrete, comprising a number of
characteristics of parameters obtained from different tests. A commonly used definition is: “that
property of freshly mixed concrete or mortar which determines the ease with which it can be mixed,
placed, consolidated and finished”. Usually expressed in terms of spread diameter of a slump flow test
(see flowability).
yield stress: A critical shear stress value below which an ideal plastic (Bingham-plastic) or viscoplastic
material behaves like a solid (i.e., will not flow). Once the yield stress is exceeded, a plastic material
yields (deforms plastically) while a viscoplastic material flows like a liquid. For non-ideal viscoplastic
materials (e.g. concrete), where the yield stress is indefinite, an apparent yield stress can be defined by
extrapolation from the linear shear rate of the flow curve to the shear stress axis (see Bingham model).
Z-potential: A suspended charged particle in a solution attracts ions of opposite charge to those at its
surface, where they form the Stern layer. To maintain the electrical balance of the suspending fluid, ions
of opposite charge are attracted to the Stern layer. The potential at the surface of the part of this diffuse
double-layer of ions that can move with the particle when subjected to a voltage gradient is the zeta-
potential. The magnitude of the Z-potential is approximately proportional to the surface charge on the
particle.
References:
Bartos P., “Fresh concrete: Properties and tests”, Department of Civil Engineering, Paisley College,
Scotland, 1992.
Bentur A., “Terminology and definitions”, RILEM report 25: Early Age Cracking in Cementitious
Systems, RILEM TC181-EAS, pp. 13-15, 2002.
EFNARC, “Specifications and guidelines for self-compacting concrete”, European Federation for
Specialist Construction Chemicals and Concrete Systems, Farnham, 2002.
EFNARC , “European guidelines for self-compacting concrete: Specification, production and use”,
European Federation for Specialist Construction Chemicals and Concrete Systems, Farnham, 2005.
Hackley V. A., Ferraris C. F., “Guide to rheological nomenclature: Measurements in ceramic
particulate systems”, NIST special publication, No 946, National Institute of Standards and
Technology, Washington, 2001.
Hackley V. A., Ferraris C. F., “The Use of Nomenclature in Dispersion Science and Technology”,
NIST publication No 960-3, Washington, 2001.
Holt E.E., “Early age autogenous shrinkage of concrete”. Technical Research Centre of Finland,
VTT Publications 446, 2001.
Jensen O.M., “Autogenous phenomena in cement-based materials”, Department of Building
Technology and Structural Engineering, Aalborg University, Denmark, 2005.
Jillavenkatesa A., Dapkunas S.J., Lum L-S.H., “Particle Size Characterization”, NIST, Puplication
No 960-1, Washington, 2001.
Lura P., “Autogenous deformation and initial curing of concrete”, Technical University of Delft,
Netherlands, 2003.
Mehta K.P., Monteiro P.J.M., “Concrete: Structure, properties, and materials”, 3rd Ed., McGraw-
Hill, 1993.
Mindess S., Young J.F., Darwin D.,”Concrete”, 2nd ed., Pearson Education Inc., 2003.
Swedish Concrete Association, “Self-compacting concrete -Recommendations for use”, Report No.
10, Svenska Betongföreningen, 2002.
Tattersall G.H., Banfill P.F.G., “Rheology of fresh concrete”, Pitman, London, 1983.
Tattersall G.H., “Workability and quality control of concrete”, E&FN Spon, London, 1991.
Tazawa E-I., ”Autogenous Shrinkage of Concrete”, Taylor and Francis, 1999.
Esping O., “Slump flow values vs. Bingham parameters for high flowable mortars and
concretes”, Accepted for publication at 5th International RILEM Symposium on Self-
Compacting Concrete, 3-5 September 2007, Ghent, Belgium, 2007.
Paper I - Slump flow values vs. Bingham parameters
for high flowable mortars and concretes
Paper I - Slump flow values vs. Bingham parameters
for high flowable mortars and concretes
Abstract
In the present work, the influence of Bingham rheology parameters on the slump flow
values of self-compacting concrete and mortar has been evaluated. The objective was to
present experimental results, without any physical validation, addressing the complex
connection between the slump flow spread, flow time (T50), yield stress and plastic
viscosity. A large number of more or less self-compacting mortars (~200 mixtures) and
concretes (~550 mixtures) with a wide range of consistency have been used for the
evaluation.
The mortar rheology was measured using a Bohlin CVO200 rheometer with concentric
setup, and the slump flow spread was measured using a mini-cone. For the concrete a
ConTec Visco5 rheometer was used together with a traditional Abram´s cone.
The results showed a large scatter and poor correlation, but a clear tendency was found.
The results indicate that the slump flow spread and T50 time are not a unique function of
yield stress or viscosity, respectively, but rather a more complex function of both. The
spread proved to be more closely connected with the yield stress than with the viscosity,
especially at high viscosity, whereas the T50 time was more dependent on both viscosity and
yield stress.
1. INTRODUCTION
To quantify the workability of fresh concrete, numerous tests of different types, more or
less empirical, have been developed. The oldest and most frequently used test today is the
slump cone test, which, associated with the Abram’s cone, has its origin in the USA around
1910 [1]. For high-flowable concrete, such as self-compacting concrete (SCC), the slump
cone is used to measure the spread of the concrete (slump flow) and the time for the concrete
to reach a spread of 500 mm (T50). For a more scientific approach, a rheometer/viscometer
can be used. The most established parameters used to define the concrete rheology are the
yield stress and plastic viscosity by the Bingham equation [2]. These rheological parameters,
unlike the measures of qualitative tests (e.g. the slump), are fundamental physical quantities,
mutually independent and not dependent on operator or equipment. But
rheometer/viscometer tests are often expensive, immobile, and mainly for laboratory use. In
the field, e.g. at concrete plant or construction site, fast, simple and cheap tests are preferred;
thus slump/slump flow and other empirical tests can hardly be replaced by a rheological test,
but should rather be a complement. To describe the flow properties of concrete, especially
for types with high flowability, a minimum of two independent parameters is required [2]-
[7]. Concrete mixtures with identical measures from an empirical test (e.g. slump flow) can
be very different in their flow behaviour. These differences can be detected by a rheological
test. However, in order to determine the properties of a non-Newtonian fluid, as all
1
Paper I - Slump flow values vs. Bingham parameters
for high flowable mortars and concretes
cementitious materials are, a multipoint flow curve has to be measured. A single point
measurement does not describe these materials correctly (see Figure 1).
Shear stress, σ
Shear stress, σ
Shear stress, σ
Viscosity
(plastic), ηpl Yield stress, σ0
It has been shown by many that the empirical tests to some extent provide information
about the concrete rheology. Slump has for a long time [3][6]-[22] been considered to be a
function of yield stress, without influence by plastic viscosity. When analysed, the density of
the concrete is often incorporated as well as the geometry of the cone. More recently the
horizontal flow spread rather than the vertical slump has been used to calculate the yield
stress [2][23]-[25]. Usually these correlations concern concretes in a small range of
flowability (e.g. HPC, SCC, etc.), and are not valid for other or wider ranges. The increased
usage of high-flowable concretes has also raised the interest in more dynamic measures such
as flow time and viscosity. The flow time can be measured by e.g. a V-funnel or L-box, but
also by measuring the time for the concrete to spread 500 mm (T50). For SCC, the slump
flow spread is generally considered to correlate with the yield stress and T50 or V-funnel
with the viscosity [26]-[28]. Often the correlation is purely empirical, but there are also some
physical models proposed to explain this relationship. Examples of physical models linking
yield stress (σ0) to slump flow spread diameter (D) are:
2 ⋅ ρ ⋅ g ⋅V
σ0 = = a / D2 (Eq. 1) [14]
π ⋅D 2
4 ⋅ ρ ⋅ g ⋅V
σ0 = = b / D2 (Eq. 2) [29]
3 ⋅π ⋅ D 2
225 ⋅ ρ ⋅ g ⋅ V 2
σ0 = = c / D 5 (Eq. 3) [30]
4 ⋅π ⋅ D
2 5
where ρ is the material density, V the sample volume and g the gravity, while a, b and c are
constants for a given sample volume and density.
The objective of this paper is not to find a physical relationship between slump flow
values and Bingham parameters, but merely to present experimental results addressing the
interaction between the slump flow spread, flow time (T50), yield stress and plastic
viscosity.
2. TEST METHODS
2
Paper I - Slump flow values vs. Bingham parameters
for high flowable mortars and concretes
millimetre. In addition to the slump flow, the time from lifting the cone to when the flow
spread reaches a 500 mm circle was recorded; referred to as T50 and stated in seconds.
Spread Spread
T50 time
diameter diameter
Figure 2: Illustration of slump flow test used for mortar and for concrete (from [31]).
2.2 Rheology
For mortar a Bohlin CVO200 rheometer was used and for concrete a ConTec Visco5, both
using a rotating concentric setup at a controlled shear rate ( γ& ) at 20ºC. The experimental
geometry and measuring sequence is illustrated in Figure 3. The two rheological parameters
plastic viscosity (ηpl) and yield stress (σ0) were evaluated in accordance with the Bingham
model: σ = σ 0 + γ& ⋅ η pl (Eq. 4).
60 Mortar sample
Shear rate [1/s]
No logging
40
Logging H=37.5 mm
Rotating and
20 measuring
inner cylinder
0 Ri=10 mm Fixed outer
0 10 20 30 40 50 60 Ro=15 mm cylinder
Time [s]
8 Ro=145 mm
Concrete
Ri=100 mm sample
Shear rate [1/s]
4
No logging H=140 mm
2 Logging Measuring
inner cylinder
0 Rotating
0 10 20 30 40 50 60 outer cylinder
Time [s]
Figure 3: The measuring sequence for the Bingham evaluation (followed by segregation
estimation) and schematic illustration of the rheometers. For mortar the Bohlin
CVO200 and for concrete the ConTec Visco5 (from [31]).
The mixes and their constituents, as used in this study, comprise typical materials for self-
compacting concrete (SCC) in Sweden. For mortar the maximum grain size was 1.0 mm, and
for concrete 16 mm.
The consistency in some cases was very stiff, but as all mixtures incorporated both filler
and superplastisizer they were considered to be self-compacting. All mixtures have their
origin in other projects whose primary purpose was to examine the effect of different
constituent properties and proportions on the rheology. Examples of this are the effect of:
w/c, cement, silica, fly ash, different limestone fillers, coarse and fine aggregate content,
superplasticizer, air entrainer, viscosity modifier, etc.
3
Paper I - Slump flow values vs. Bingham parameters
for high flowable mortars and concretes
The mortar samples were prepared in batches of 0.5-1.0 litres, using a 4.73 litre Hobart
laboratory paddle mixer. The mixing sequence was based on ASTM C305 standard. The
concretes were prepared in batches of 30-60 litres, mixed in a BHS60 twin-shaft paddle
mixer for 4 minutes after water was added to the premixed dry materials. The admixtures
were added directly after the water.
4
Paper I - Slump flow values vs. Bingham parameters
for high flowable mortars and concretes
70 600
>350 mm >700 mm
60 300-350 mm 600-700 mm
500
250-300 mm 500-600 mm
200-250 mm 200-300 mm 400-500 mm
50
150-200 mm
400 300-400 mm
Yield stress [Pa]
100-150 mm 300
30 300-400 mm
150-200 mm
200
20
200-250 mm 400-500 mm
10 250-300 mm 100
500-600 mm
300-350 mm
>350 mm 600-700 mm
0 >700 mm
0
0 2 4 6 8 0 50 100 150 200
Viscosity [Pa s] Viscosity [Pa s]
Figure 4: The slump flow spread (in intervals of 50 resp. 100 mm) and Bingham rheology
parameters (yield stress and plastic viscosity) for the mortar and concrete.
Based on all the investigated mixes (> 750 mixes), the following approximate model for
calculating the relative slump flow area (Rp) for both mortar and concrete is proposed:
( H / 6 )2
Rp ≈ (Eq. 5) R p = ( D / D0 ) 2 − 1 (Eq. 6)
ln( η pl + 2 ) ⋅ σ 0
where ηpl is the plastic viscosity, σ0 the yield stress, H the cone height (60 resp 300 mm), D
the measured spread diameter in millimetre and D0 the flow cone bottom diameter (100 resp
200 mm). The model is purely empirical and is deficient in its units. In Figure 5 the model is
plotted for mortar and concrete.
70 600
60 Mortar Concrete
50
Yield stress [Pa]
Yield stress [Pa]
400
40 200-300 mm
100-150 mm
30
200 300-400 mm
20
150-200 mm
200-250 mm 400-500 mm
10 250-300 mm 500-600 mm
300-350 mm 600-700 mm
>350 mm >700 mm
0 0
0 2 4 6 8 0 50 100 150 200
Viscosity [Pa s] Viscosity [Pa s]
In Eq.5 the yield stress is predominant, where the effect of a change in yield stress
corresponds to ~3 times larger change in viscosity on the slump flow. These differences are
smaller at low viscosity, and are independent of the magnitude of yield stress.
In the literature, not all studies agree that slump flow spread is a measure of concrete
yield stress. For example, Nielssen & Wallevik [32] explain how a low viscosity will increase
the downward speed, overcome the yield stress and thereby generate a large slump flow
5
Paper I - Slump flow values vs. Bingham parameters
for high flowable mortars and concretes
spread. For high viscosity the effect will be the opposite. Cauberg et al [33] state that the
relation between yield stress and slump flow, without taking viscosity into account, does not
show a satisfactory fit, and that these relations usually are formed for a certain range of
fluidity. Furthermore, a variable Z0, comprising both yield stress (σ0) and viscosity (ηpl), is
proposed for a better fit to the slump flow spread (D) in millimetres.
Z 0 = a ⋅ σ 0 + b / η pl (Eq. 7) Z 0 = 381 − 0.586 ⋅ D (Eq. 8)
where a and b are constants. In the region of spread D=400-600 mm, and with a=1 and
b=1000, Eq. 7 and Eq. 8 generate similar results as Eq. 5 and Eq. 6. For spread D>650 mm
Eq. 8 is not valid. Furthermore, the shape of the curve in a ηpl-σ0 diagram is independent of
the spread. Smeplass [34] has noted that the slump is more related to the yield stress than to
the viscosity of concrete, while the flow table spread is more related to the viscosity than the
yield stress. If the viscosity varies, at constant yield stress, so will the flow measures.
80
2-4 s
<2
>10 s
8-10 s
40
4-6 s 6-8 s
2-4 s
<2 s
0
0 50 100 150
Viscosity [Pa s]
Figure 6: The experimental results of slump flow spread time T50 (in intervals of 2 s) and
Bingham rheology parameters (yield stress and plastic viscosity) for the
concrete.
Based on the results, the following empirical model for calculating the slump flow spread
time T50 in seconds is proposed:
T 50 ≈ 0.002 ⋅ σ 0 ⋅ η pl (Eq. 9)
In the literature, there is no general agreement that T50 is a measure of concrete plastic
viscosity (ηpl). For example, Tedaka et al [35] state that the slump flow spread corresponds
well to the yield stress (σ0), whereas the T50 flow time does not alone represent the viscosity
since slump flow also contributes. Thus, T50 can be used to evaluate the viscosity only when
the slump flow is constant. Furthermore, Ferraris et al [36] show that the slump flow spread
times of cement pastes with a wide range of yield stress have no correlation at all with the
viscosity. Emborg [37] has also noted a weak correlation, but then for the T50 vs. viscosity
6
Paper I - Slump flow values vs. Bingham parameters
for high flowable mortars and concretes
of SCC. Utsi et al [38] have observed that T50 correlates not only to the viscosity but also to
the yield stress, and proposes that both the yield stress and viscosity influences the T50 and
slump flow respectively. By dividing the slump flow into different intervals the correlation
between T50 and viscosity was shown to be acceptable, which further fortified this theory.
5. CONCLUSIONS
It has been shown by many investigators that the results of empirical tests are strongly
related to the concrete rheology. For SCC, the slump flow spread is generally considered to
be a function of yield stress and T50 or V-funnel of viscosity. Often this correlation is purely
empirical, but there are also different physical models explaining this relationship. In the
presented work, the influence of Bingham rheology parameters on the slump flow values of
a large number of more or less self-compacting concrete and mortar has been evaluated.
Experimental results addressing the connection between the slump flow spread, flow time
(T50), yield stress and plastic viscosity are presented. The results clearly indicate that the
slump flow spread and T50 time are not a unique function of yield stress and viscosity
respectively, but rather a more complex function of both where neither yield stress nor
viscosity can be neglected. The spread proved to be more closely connected with the yield
stress than the viscosity (~3 times), especially at high viscosity, whereas the T50 time was
connected more equally with yield stress and viscosity. Consequently, T50 can only be used
to estimate the viscosity for mixture with constant yield stress, and slump flow can only be
used to estimate the yield stress with constant viscosity.
ACKNOWLEDGEMENTS
Financial support from Thomas Concrete Group and Färdig Betong is greatly appreciated.
REFERENCES
[1] Bartos P., Sonebi M., Tamimi A. K. (2002): “Workability and rheology of fresh concrete:
Compendium of tests”, RILEM, France.
[2] Tattersall G.H. (1991): “Workability and quality control of concrete”, E&FN Spon, London.
[3] Domone P. (1998): ”The slump flow test for high-workability concrete”, Cement and Concrete
Research, vol 28(2), pp 177-182.
[4] Domone P.L.J., Xu Y., Banfill P.F.G. (1999): “Developments of the two-point workabiliy test
for high-performance concrete,” Magazine of Concrete Research, Vol 51(3), pp 171-179, 1999.
[5] Ferraris C.F., “Measurement of the rheological properties of high performance concrete: State
of art report”, Journal of NIST, vol 104(5), pp 461-478.
[6] Tattersall G.H. (1973): “The rationale of a two-point workability test,” Magazine of Concrete
Research, vol 25 (84), pp 169-172.
[7] Tattersall G.H., Banfill P.F.G. (1983): “Rheology of fresh concrete”, Pitman, London.
[8] Chidiac S.E., Madaani O., Razaqpur A.G., Mailvaganam, N.P. (2000): “Controlling the quality
of fresh concrete - A new approach”, Magazine of Concrete Research, vol 52 (5), pp 353-364.
[9] Clayton S., Grice T.G., and Boger D.V. (2003): “Analysis of the slump test for on-site yield
stress measurement of mineral suspensions”, Journal of Mineral Processing, Vol 70, pp 3-21.
[10] de Larrard F. (1999): “Concrete mixture proportioning, a scientific approach”, F&FN Spon,
New York.
[11] de Larrard F., Hu C., Sedran T., Szitkar J.C., Joly M., Claux F., Derkx F. (1997): “A new
rheometer for soft-to-fluid fresh concrete”, ACI Materials Journal, vol 94(3), pp 234-243.
[12] Ferraris C.F., de Larrard F. (1998): “Testing and modelling of fresh concrete rheology”,
NISTIR 6094, NIST, USA.
[13] Hu C., de Larrard F., Sedran T., Boulay C., Bosc F., Deflorenne F. (1996): “Validation of
BTRHEOM, the new rheometer for soft-to-fluid concrete”, Materials and Structures, vol
29(194), pp 620-631.
7
Paper I - Slump flow values vs. Bingham parameters
for high flowable mortars and concretes
[14] Murata J. (1984): “Flow and deformation of fresh concrete”, Materials and Structures, vol
17(98), pp 117-129.
[15] Murata J., Kikukawa H. (1992): “Viscosity Equation for Fresh Concrete”, ACI Materials
Journal, vol 89(3), pp 230-237.
[16] Norberg J., Peterson O., Billberg P. (1997): “Effects of a new generation of superplasticizers on
the properties of fresh concrete”, CANMET/ACI International Conference, pp. 583-598, Italy.
[17] Pashias N., Boger D.V., Sumers J., Glenister D.J. (1996): “A Fifty Cent Rheometer for Yield
Stress Measurements”, Journal of Rheolgy, vol 40(6).
[18] Saak A.W., Jennings H.M., Shah, S.P. (2004): “A generalized approach for the determination of
yield stress by slump and slump flow”, Cement and Concrete Research, Vol 34, pp. 363-371.
[19] Schowalter W.R., Christensen G. (1998): “Toward a rationalization of the slump test for fresh
concrete -Comparisons of calculations and experiments”, J. of Rheology, vol 42(4), pp 865-870.
[20] Tanigawa Y., Mori H. (1989): Analytical study on deformation of fresh concrete”, Journal of
Engineering Mechanics, vol 115(3), pp 493-508.
[21] Tanigawa, Y., Mori, H., Watanabe, K. (1990): “Computer simulation of consistency and
rheology tests of fresh concrete by viscoplastic”, RILEM symposium on properties of fresh
concrete, pp 301-308, Hanover.
[22] Wallevik J. E. (2006): “Relationship between the Bingham parameters and slump”, Cement and
Concrete Research, vol 36, pp 1214-1221.
[23] Flatt R.J., Domenico L., Roussel N. (2006): “Linking yield stress measurements: Spread test
versus Viscomat”, Cement and Concrete Research, vol 36(11), pp 99-109.
[24] Rossel N., N’Guyen H.T.L., Coussot P. (2005): “Yield measurements using stoppage tests”,
RILEM symposium on SCC, pp 575-582, Chicago.
[25] Saak A.W., Jennings H.M., Shah S.P. (2004): “A generalized approach for the determination of
yield stress by slump and slump flow”, Cement and Concrete Research, vol 34(3), pp 363-371.
[26] Domone P.L. and Jin J. (1999): “Properties of mortar for self-compacting concrete” RILEM
symposium on SCC, pp 109-120, Stockholm.
[27] Grünewald S., Walraven J.C. (2003): “Rheological measurements on self-compacting fibre
reinforced concrete”, RILEM Symposium on SCC, PRO 33, pp 49-58, Reykjavik.
[28] Jin J., Domone P.L. (2002): “Relationships between the fresh properties of SCC and its mortar
component”, North American Conference on the Design and Use of Self-Consolidating
Concrete, pp 33-38, Chicago.
[29] Chidiac S.E., Maadani O., Razaqpur A.G., Mailvaganam N.P.(2000): ”Controlling the quality
of fresh concrete - a new approach”, Magazine of Concrete Research, vol 52(5), pp 353-363.
[30] Roussel N., Stefani C., Leroy R.,” From mini-cone test to Abrams cone test: measurement of
cement-based materials yield stress using slump tests”, Cement and Concrete Research, vol
35(5), pp 817-822.
[31] Esping, O. (2004): “Rheology of cementitious materials: effects of geometrical properties of
filler and fine aggregate”, Report 04:3, Chalmers University of Technology, Göteborg.
[32] Nielsen I., Wallevik O.H. (2003): “Rheological evaluation of some empirical test methods –
Preliminary result”, RILEM symposium on SCC, pp 55-68, Reykjavik.
[33] Cauberg N., Desmyter J., Dieryck V. (2005): “Rheology of Self-Compacting Concrete -
Validation of Empirical Test Methods”, RILEM symposium on SCC, pp 765-773, Chicago.
[34] Smeplass S. (1993): “Applicability of the Bingham model to high strength concrete”, RILEM
workshop on special concretes – Workability and mixing, pp 145-151, Paisley.
[35] Takada K., Tangtermsirikul S. (2000): “Testing of Fresh Concrete”, Self-compacting concrete:
State-of-the-art report, RILEM Technical Committee 174-SCC, Report 23, pp 25-39, France.
[36] Ferraris C., Obla K., Hill R. (2001): “The influence of mineral admixtures on the rheology of
cement paste and concrete”, Cement and Concrete Research, Vol 31(2), pp 245-255.
[37] Emborg M. (1999): “Rheology tests for self-compacting concrete - How useful are they for the
design of concrete mix for full scale production?”, RILEM symposium on SCC, pp 95-105,
Stockholm.
[38] Utsi S., Emborg M., Carlswärd J. (2003): “Relation between workability and rheological
parameters”, RILEM Symposium on SCC, PRO 33, pp 154-164, Reykjavik.
8
Paper II - Methods for characterisation
of fillers and fines for SCC
Esping O., “Methods for characterisation of fillers and fines for self-compacting
concrete”, 3rd International RILEM Symposium on Self-Compacting Concrete, PRO 33,
17–20 August, pp 208-219, Reykjavik, Iceland, 2003.
Paper II - Methods for characterisation
of fillers and fines for SCC
Paper II - Methods for characterisation
of fillers and fines for SCC
Oskar ESPING
Chalmers University of Technology, Sweden
ABSTRACT: Due to the large surface area, quantification of fillers and the fine part of
aggregates is essential for the ability to control physical properties, such as workability of
self-compacting concrete. A new simple method for measuring the surface area has been
investigated and compared with other traditional methods.
The properties of eight different fillers (seven limestone and one glass filler) and their
influence on the rheology of self-compacting mortar have been evaluated.
1. INTRODUCTION
The rheology of a particle suspension is a function of the suspending media. For concrete,
optimized size distribution influence the workability positively since the suspension consists
of a matrix where the suspension of smaller particles fills the hollow spaces between the
coarser. To decrease the internal friction of fresh concrete, the particle surface is to be
covered with water and voids in the system to be filled. More water will reduce the volume
fraction of particles and thereby eases the particle motion. Consequently, when the contact
zone between the particles decreases there will be a significant reduction of plastic viscosity
and yield stress [1,2,4]. Besides particle concentration and size distribution, other important
properties affecting the workability are particle shape, porosity and surface texture [3].
So, due to the large surface area, quantification of geometrical properties of fillers and the
fine part of the aggregates is essential for the ability to control physical properties, such as
workability, in the production of self-compacting concrete (SCC).
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Paper II - Methods for characterisation
of fillers and fines for SCC
In this study, the properties of eight different fillers (seven limestone and one glass filler)
and their influence on the rheology of self-compacting mortar have been evaluated.
Traditional methods for measuring the surface area has been investigated and compared with
a new simple method, called BET (H2O).
2.2 Methodology
The BET (H2O) is based on BET theory (named after Brunauer, Emmett and Teller) [8]
where the specific external surface area is estimated from determining the quantity of a
specific gas that adsorbs as a single layer of molecules, a so-called monomolecular layer,
under controlled conditions. But instead, as normally, of using nitrogen gas at controlled
temperature and pressure, moisture at two ore more relative humidity (RH) levels are used.
The technique by using the BET-relation with moisture instead of nitrogen gas has been
applied by Fuglsang Nielsen [6] and Ahlgren [7], but the focus was on internal porosity and
not on external particle surface.
It ought to be noted that moisture adsorption is not the same as for nitrogen gas. The water
molecule is slightly smaller than the nitrogen molecule, and the water molecule has larger
affinity forces (attraction) due to its two-polar covalent bonds (see Figure 2 and Figure 3).
However, using water (moisture) is probably closer to real condition in concrete production
than using nitrogen gas.
To be able to use the BET theory with moisture as an adsorbent restricted to a
monomolecular layer, the vapour pressure must be low. Therefore the RH is limited to
approximately 30% (at 20ºC).
Adsorbed +
H
molecules
+ N N
H O
-
Mono-layer
(~3.5Å for water) H 2O N2
When evaluating the BET (H2O)-method, a "two pressure" humidity generator (Thunder
2500, see Figure 4) where the specimens were conditioned in air vaporized at several levels
2
Paper II - Methods for characterisation
of fillers and fines for SCC
(6, 12, 16, 20, 25, 30 and 50% RH) with high accuracy. This was then compared with a
method where the specimens were conditioned in two separate climate boxes (11.3 and
33.1% RH with LiCl and MgCl2 salt, see Figure 5). The climate box (salt) method showed
adequate results, and are due to its simplicity a recommended method.
Figure 4. The Thunder 2500, a Figure 5. Two climate boxes with RH 11% (LiCl) and
"two pressure" principle humidity 33% (MgCl2) For stable atmospheres, the box must be
generator, producing tight and a mechanical fan are to be rotate the air
atmospheres with high accuracy. inside. The temperature must be kept constant at 20ºC.
STP [kg/kg]
as a function of the relative humidity RH, the variables a and
b can be calculated by a linear relationship (see Figure 6).
The specific area S is then calculated according to Eq.3. [7] b
RH a
STP = [kg/kg] (RH {0;1}) (Eq.1)
(u ⋅ (1 − RH )) RH [-]
3. EXPERIMENTAL SETUP
3.1 Quantification methods
3.3.1 Surface area from size distribution
The surface area of the fillers was calculated from the particle size distribution, both from
the laser diffraction analyze (given in Figure 12) and from the image analysis (see section
3.3.5.), assuming spherical particles. The size distribution from the image analyze was
determined according to the Nordtest method NT BUILD 486.
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Paper II - Methods for characterisation
of fillers and fines for SCC
The method is described in chapter 2.2. The test was performed both by Norkalk AB (lime-
stone filler producer) using a Micromeritics BET analyzer and by SP (Swedish National
Testing and Research Institute) also using a Micromeritics.
3.3.4 Blaine
The method determines fineness of powders in terms of specific surface. The test was made
according to ASTM C204 standard, with a Tonindustrie instrument. Norkalk AB also
performed this test, using a ToniPerm instrument.
F-shape: the ratio of the length of the minor axis (Dmin) to a) Dmin
the length of the major axis (Dmax). If the elongation is 1, Dmax
the object is roughly circular or square (see Figure 7). The
F-shape is computed as:
Dmin / Dmax [-] (Eq.4)
b) Area p. Perimeter
F-circle: the ratio of measured area and area of a circle with
Area c.
the same perimeter as measured. At 1, the object is circular
(see Figure 7). The F-circle is computed as:
4 ⋅ π ⋅ Area
[-] (Eq.5)
Perimeter 2 c)
Dmax
Compactness: the ratio between the diameter of a circle
with the same area as measured (Dcircle) and the maximum Dcircle
elongation (Dmax) of measured area and. At 1, the object is
circular (see Figure 7). The Compactness is computed as:
Figure 7. a) F-shape; b)
2 ⋅ Area / π F-circle; c) Compactness.
[-] (= Dcircle / Dmax) (Eq.6)
Dmax
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Paper II - Methods for characterisation
of fillers and fines for SCC
( D 2 − D02 )
Rp = 2
[m2/m2] (Eq.7)
D0
Vw/Vp [-]
70 mm
D is the average spread diameter, calculated in
four directions and D0 is the base diameter of Ep
60 mm
cone (Figure 8).
βp
D0 = 100 mm
The measure of retained water ratio βp can be Rp [-] D D 3 4
considered as the amount of water, adsorbed D
1
D 2
3.4.2 Rheology
A Bohlin CVO200 rheometer with rotating coaxial
cylinder was used to measure plastic viscosity (ηpl),
yield stress (σ0) and thixotropy at controlled shear
rate ( γ& ). The measuring device consisted an outer
cylinder (cup) with diameter Do=30 mm and a
grooved inner cylinder (bob) with diameter Di=20
mm, providing a gap of 5 mm (see Figure 10). The
temperature was controlled and kept constant at
20±0.1°C. The evaluation of viscosity and yield
stress was made according to the Bingham model
(see Eq.8) and the thixotropy was evaluated from a
linear up/down loop where the area in the flow
curve represented the thixotropic measure.
σ = σ 0 + γ& ⋅ η pl (Eq.8)
The measuring sequence setup was made after Figure 10. Bohlin CVO200 rheometer
consultation with Dr O. Wallevik [11] and is shown with a grooved inner cylinder (bob).
in Figure 11.
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Paper II - Methods for characterisation
of fillers and fines for SCC
50 Logging
Shear stress, σ [Pa]
No logging 1
40
2
Shear rate [1/s]
20 1 2 3 Thixotropy [Pa/s]
10 Viscosity,ηpl [Pa s]
Figure 11. The measuring sequence setup with a first loop (1) measuring the thixotropy, a
second (2) for the Bingham evaluation and a third (3) for segregation estimation.
Table 2. Materials.
Material Type Name Supplier Age Density
[milj years] [kg/m3]
Cement: CEMII/A-LL42,5R Byggcement (Bygg) Cementa 2980
Aggregate: Sand Baskarpsand 15 (B15) Baskarpsand 2650
Filler: Limestone Limus 10 (L10) Nordkalk 500 2680
Limestone Limus 15 (L15) Nordkalk 80 2710
Limestone Limus 25 (L25) Nordkalk 1900 2710
Limestone Limus 40 (L40) Nordkalk 1900 2670
Limestone Limus 180 (L180) Nordkalk 500 2740
Limestone L180X Nordkalk 1900 2730
Limestone Limus 190 (L190) Nordkalk 80 2700
Returned glass MicroFiller SGÅ 2510
Plasticizer: Polucarboxylate Sikament-56 Sika 1100
The mortar recipe is based on a "normal" (in Sweden) SCC, where the proportions were
scaled down due to the maximum grain size 0.5 mm.
The volume of aggregate, cement and plasticizer were kept constant, while the w/c was
varied in tree levels 0.45, 0.50 and 0.55. The volume distribution of the recipes is shown in
Figure 14. Due to different filler density, totally 24 recipes were produced. Each mortar mix
was prepared according to the ASTM Standard C 305 at 20˚C.
6
Paper II - Methods for characterisation
of fillers and fines for SCC
L190
60
Passing [%]
MF
L40
Bygg MF Figure 12.
B15
40
L190
Size distribution
of the seven
20
L180X
limestone fillers
and the glass
B15
filler measured
0 with a Malvern
0,002 0,004 0,008 0,016 0,031 0,063 0,125 0,250 0,500 laser diffraction
Size [mm]
instrument.
Figure 13. Pictures of the fillers, taken with scanning electron microscope (SEM). The edge
length of each picture responds to 0.5 mm. The specimens are epoxy-mould and polished.
Cement Cement
Water Cement
25,0% Water Water 25,0%
33,5% 25,0%
37,2% 41,0%
Aggregate Aggregate
Aggregate
Filler 25,0%
25,0% 25,0%
Filler
16,1% Filler
12,4%
8,7%
w/c 0.55
w/c 0.45 w/c 0.5
Figure 14. Mix proportion by volume.
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Paper II - Methods for characterisation
of fillers and fines for SCC
700 10000
Calculated (Size distr)
600
BET (N)
Calculated (SEM) 8000
500 BET (H2O)
Blaine
400 6000
300 4000
200
2000
100
0 0
X
X
80
90
F
0
80
90
80
80
L1
L1
L2
L4
L1
L1
L2
L4
M
M
L1
L1
L1
L1
L1
L1
Figure 15. Specific area calculated from size Figure 16. Specific area measured with
distribution and measured with Blaine. BET (N) and BET (H2O).
Vw/Vp
Geometry Retained water and sensitivity
F-shape
0,9
F-circle Ep
0,06 1,00
Compactness βp
R
0,05
0,8
retained water ratio βp [-]
F -s hape, F -c irc le and
Ep 0,80
Com pac tnes s [-]
0,05
Bp
0,04
0,7
0,60
0,04
0,6 0,03
0,40
0,03
80
90
F
0
F
X
80
90
80
L1
L1
L2
L4
M
L1
L1
L2
L4
M
80
L1
L1
L1
L1
L1
L1
Figure 17. Roundness factors as F-shape, F- Figure 18. Retained water and sensitivity.
circle and Compactness, measured and Note that a high deformation coefficient
calculated from Image analysis (SEM). indicates a sensitive material.
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Paper II - Methods for characterisation
of fillers and fines for SCC
w/c 0,55
100
10
1 0
X
0
0
X
F
80
90
0
F
80
90
80
L1
L1
L2
L4
L1
L1
L2
L4
80
M
M
L1
L1
L1
L1
L1
L1
Figure 19. Yield stress σ0 for the w/c 0.45, 0.50 Figure 20. Plastic viscosity ηpl for the w/c
and 0.55 mortar mix. 0.45, 0.50 and 0.55 mortar mix.
Rheology Rheology
10000 400
w/c 0,45 w/c 0,45
w/c 0,50 350 w/c 0,50
1000 w/c 0,55 w/c 0,55
Slump flow D [mm]
Thixotropy [Pa/s]
300
100 250
200
10
150
1 100
X
X
0
0
F
F
80
90
80
90
L1
L1
L2
L4
80
80
L1
L1
L2
L4
M
M
L1
L1
L1
L1
L1
L1
Figure 21. Thixotropy for the w/c 0.45, 0.50 Figure 22. Slump flow diameter D for the w/c
and 0.55 mortar mix. 0.45, 0.50 and 0.55 mortar mix.
4.3 Correlation
A correlation analyze was performed with the software tool AXUM 6.0. The results are
listed in Table 3, The correlation coefficient is represented by the Pearson product moment
corre-lation r, calculated as:
n ⋅ ∑ ( x ⋅ y ) − ∑ x ⋅∑ y
r= [-] (Eq.9)
(
n ⋅ ∑ x 2 −( ∑ x ) 2 ⋅ n ⋅ ∑ y 2 − ( ∑ y ) 2 )( )
x and y are the variables and n is the number of pairs that are to be compared.
The greater value of r the stronger correlation, as follows:
0.8 - 1.0 very strong
0.6 - 0.8 strong
0.4 - 0.6 moderate
< 0.4 weak
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Paper II - Methods for characterisation
of fillers and fines for SCC
There are also negative relations, but the important quality of correlation coefficients is not
their sign, but their absolute value.
Table 3. Correlation matrix within geometry and between geometry and rheology. Results
with "very strong" (>0.8) correlation are typed bold and the strong (0.6 - 0.8) are
underlined.
Asize ASEM BETN BETH2O Blaine F-shape F-circle Comp. Ep βp
Asize 1.00
ASEM 0.84 1.00
BETN 0.49 0.21 1.00
BETH2O 0.32 0.08 0.98 1.00
Blaine 0.94 0.77 0.47 0.30 1.00
F-shape 0.23 -0.12 0.62 0.58 0.43 1.00
F-circle 0.25 -0.22 0.68 0.65 0.34 0.87 1.00
Comp. 0.49 0.02 0.79 0.72 0.54 0.85 0.95 1.00
Ep 0.88 0.60 0.76 0.62 0.90 0.57 0.54 0.75 1.00
βp 0.44 0.35 0.73 0.75 0.54 0.47 0.41 0.45 0.61 1.00
Thixotr. 0.13 0.00 0.81 0.89 0.15 0.41 0.49 0.47 0.38 0.86
w/c 0.45
σ0 0.35 0.07 0.86 0.84 0.42 0.54 0.66 0.70 0.67 0.76
ηpl 0.34 0.17 0.80 0.82 0.40 0.43 0.55 0.55 0.56 0.90
D -0.26 -0.19 -0.70 -0.75 -0.33 -0.38 -0.44 -0.40 -0.42 -0.94
Thixotr. 0.08 -0.02 0.65 0.71 0.18 0.33 0.43 0.37 0.34 0.83
w/c 0.50
σ0 0.37 0.08 0.95 0.93 0.41 0.60 0.69 0.75 0.71 0.75
ηpl 0.33 0.19 0.81 0.83 0.41 0.45 0.50 0.52 0.58 0.92
D -0.30 -0.19 -0.80 -0.84 -0.37 -0.47 -0.50 -0.50 -0.52 -0.94
Thixotr. 0.35 0.30 0.52 0.55 0.41 0.12 0.20 0.22 0.43 0.88
w/c 0.55
σ0 0.42 0.24 0.87 0.84 0.47 0.41 0.49 0.58 0.69 0.82
ηpl 0.46 0.37 0.62 0.64 0.48 0.18 0.28 0.32 0.52 0.92
D -0.41 -0.37 -0.74 -0.75 -0.44 -0.23 -0.27 -0.34 -0.56 -0.93
But it ought to be pointed out that F-shape is more a measure of shape, F-circle more a
measure of texture and Compactness is somewhere between. This is exemplified in Figure
24 with four different geometrical shapes (ellipse, rectangle, triangle and hexagon) and their
impact on the roundness factor by changed size ratio (d/D).
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Paper II - Methods for characterisation
of fillers and fines for SCC
The quantification by image analysis was problematic. The method is strongly dependent of
a large numbers of factors, such as: sample preparing, microscope performance, photo
quality (sharpness), resolution, number of particles, analyzing software, threshold technique,
etc. The method might be better if a larger part of the procedure were automatized and
standardized.
Compactness [-]
Hexagone
Rectangle
0,6 0,6
Fcircle [-]
0,6
Fshape [-]
Triangle
Hexagone 0,4
0,4 0,4 Ellipse
Rectangle
0,2 0,2 0,2 Triangle
Hexagone
0,0
0,0 0,0
1:1 1:2 d/D 1:3 1:4 1:1 1:2 d/D 1:3 1:4 1:1 1:2 d/D 1:3 1:4
a) b) c) d)
d d d d
D D D D
Figure 24. The roundness factors F-shape, F-circle and Compactness and their geometrical
dependency exemplified by a) ellipse, b) rectangle, c) triangle and d) hexagon.
6000
not equal, the linear relationship is good (see
4000
Figure 26). One has to be aware of the
differences in size and polarity of the water and 2000
nitrogen molecule. This test has also been made 0
on fines (<1.0mm) sieved from different 0 2000 4000 6000 8000 10000 12000
aggregates, with the same good results. For BET (Nitrogen) [m2/kg]
binders, type cement, the BET (H2O) method has Figure 26. The linear correlation
not supplied reliable measures, and therefore not between the BET (N) and BET (H O)
2
recommended. measures.
Both BET (N) and BET (H2O) show strong correlation to the rheological measures. Why the
BET-method is better connected with rheological properties than the other surface area
quantifications could be explained by importance of shape, surface texture and porosity. If
11
Paper II - Methods for characterisation
of fillers and fines for SCC
the spread flow diameter D is recalculated into flow area (see Eq.4), the correlation with
BET gets even better. This is probably due to an exponential relation.
5. CONCLUSIONS
Due to the importance of the large surface area, quantification of fillers and the fine part of
aggregates properties is essential for the ability to control physical properties, such as
workability in the production of self-compacting concrete.
This study has proven the importance of particle size and geometry (shape, surface porosity
and texture).
The BET (H2O), a simple characterisation method for fillers and fines for self-compacting
concrete, has been introduced. The BET (H2O) has proven high potential. It is simple, low
cost, and has provided stable and reliable values. It has also shown on a strong correlation
with rheological properties and with the traditional BET (Nitrogen).
Other quantification methods have been carried out, but the specific area, quantified with
BET-technique, has shown to be the single most important measure concerning the mortar
rheology.
REFERENCES
1. Barnes H. A., Hutton J. F., Walters K., (1989), "An introduction to rheology", Elsevier,
Amsterdam.
2. Bartos P., (1992), "Fresh concrete: Properties and tests", Elsevier, Amsterdam.
3. Tattersall G. H., (1991), "Workability and quality control of concrete", E&FN Spon,
London.
4. Billberg P., (1999), "Self-compacting concrete for civil engineering structures - the
Swedish experience", Swedish Cement and Concrete Research Institute, CBI report 2:99,
Stockholm.
5. Persson A-L., (1996), "Image analysis of fine aggregates: Characterisation of shape and
grain-size parameters", Licentiate thesis, Royal Institute of Technology, Stockholm.
6. Fuglsang Nielsen L., (1993) "Moisture sorption in porous material - A modified BET-
description", 3rd Symposium on building physics in norden contries, pp 719-724, Vol 2,
Copenhagen.
7. Ahlgren L., (1972), "Moisture fixation in porous building materials", Devision of
building technology the Lund institute of technology, Report 36, Sweden (in Swedish)
8. Brunauer S., Emmet H. P., Teller., (1938) "Adsorption of gasses in multimolecular
layers", American Chemical Society.
9. Okamura H., Ozawa K., (1995), "Mix design for self-compacting concrete", Concrete
Library of the JSCE, No 25, pp 107-120, June, (Translation from Proc. of ISCE, No
496/V-24, 1994.8).
10. Domone P. L., Chai H., (1997), "Testing of binders for high performance concrete",
Cement and Concrete Research, Vol 27 (8), pp 1141-1147.
11. Personal communication with Dr O. Wallevik (Head of Concrete Division at the
Icelandic Building Research Institute), 2001.
12
Paper III - SCC flowability: Effect of changes in particle
surface area, and how to compensate for this
Esping O., “SCC flowability: Effect of changes in particle surface area, and how to
compensate for this”, Accepted for publication at 5th International RILEM Symposium
on Self-Compacting Concrete, 3-5 September, Ghent, Belgium, 2007.
Paper III - SCC flowability: Effect of changes in particle
surface area, and how to compensate for this
Paper III - SCC flowability: Effect of changes in particle
surface area, and how to compensate for this
Abstract
Due to the large particle surface area, quantification of fillers and the fine part of aggregates
is essential for the ability to control physical properties, such as workability of self-
compacting concrete. In the presented work, the effect of the specific surface area of gravel
and limestone filler on the rheology of self-compacting concrete has been evaluated. The
surface area was measured with a simplified BET-method, using water as adsorbate. A
model is presented, where a change in specific area by BET(H2O) is translated to a change in
water demand for the concrete mix. The model is based on an assumption that 30 full
molecular layers of water, covering the particle surface is required to decrease interactions
and provide lubrication, sufficient to create flowability. The results indicated that a change in
BET(H2O)-area of 1000 m2/kg corresponds to approximately 0.8% moisture content of the
gravel. E.g. a SCC with 1000 kg gravel (0-8 mm) that increases by 1000 m2/kg in area will
need 8.5 litre extra water, in order to retain its consistency. In cases where traditional
methods for geometrical characterization (size distribution, water absorption, modulus of
fineness, etc.) is kept within acceptance a normal gravel for concrete can vary by up to 7000
m2/kg in surface area.
1. INTRODUCTION
For concrete, particle concentration and size distribution strongly influences the workability
since its matrix consist a suspension of smaller particles filling the hollow spaces between
the coarser. To decrease the internal friction and generate mobility, the particle surfaces are
to be covered with water and the voids in the system to be filled. More water will reduce the
volume fraction of particles and thereby eases the matrix motion. Consequently, when the
contact zone between the particles decreases there will be a significant reduction of plastic
viscosity and yield stress. Other important properties affecting the workability are the
particle shape, porosity and surface texture. Since the ratio of surface area to volume
increases exponentially by particle irregularity (shape, surface texture and porosity) and
decreased size, quantification of geometrical properties of fillers and the fine part of the
aggregates is essential for the ability to control physical properties, such as workability.
A common problem at the job site or plant is that fresh concrete, of a given mix design, can
vary in workability from batch to batch and can have a large variation in consistency over
time (i.e. consistency loss). This is especially problematic for the self-compacting concrete
(SCC), due to its great complexity and because of its sensitivity to variation in the
constituents’ properties (gravel moisture content, aggregate grading, etc.). Contrary to
ordinary concrete with insufficient flowability on site, SCC is not to be adjusted with extra
water or plasticizer, or given extra energy by vibrating.
1
Paper III - SCC flowability: Effect of changes in particle
surface area, and how to compensate for this
As the aggregate represents 60-80% of the total volume of concrete, it is obvious that its
influence on the fresh and hardened concrete is substantial. It is well known that two
aggregates, with apparently similar grading, can provide significant differences in concrete
workability (see e.g. [6] and [9]). These differences can be referred to the aggregate fineness,
surface texture, shape, porosity, mineralogy, etc. Properties of fine particles (<63 µm) and
their influence are often neglected because traditional standard methods for characterizing
aggregates are deficient or too complicated. Even though the content by volume or weight is
often small, the number of particles and their total surface area are large. A content of up to 3
vol-% of particles finer than 63 µm (EN 933-1, or 75 µm according to ASTM C33) is
normally considered harmful, but these particles and their surface properties have a
considerable influence on the quality of the concrete, either fresh or in hardened state [8].
The gravel fineness is traditionally quantified by modulus of fineness from the size
distribution, a method underestimating the contribution of the fines. The cement and filler
particles fineness is traditionally quantified with Blain measure. Due to the methodology
where the specific surface area is determined from air permeability, based on packed
spherical particles, information of the shape, texture and surface porosity is neglected. Other
possibly more correct methods, such as the BET with Nitrogen gas and image analysis is
more seldom used due to its complexity and costs.
The aim of this experimental study was to investigate the possibility to detect variations in
raw material properties that are deleterious for the fresh concrete quality, and how to
compensate for these.
2. TEST METHODS
2.1 BET(H2O)
By using BET theory, the specific surface area (S) can be determined by deducing the area
from the adsorbed volume of gas molecules required to cover and form a monolayer on the
surface of the sample [3]. The filler and fine part of aggregate specific surface area was
determined gravimetrically by the BET multipoint method, using water (moisture) as
adsorbate at different relative humidity (RH). The test was performed at 20ºC with climate
boxes with 11.3% and 33.1% RH, achieved with LiCl and MgCl2 saturated salt solutions (see
Figure 1a). The sample size was approximately 100 g, the weight (m) was measured by a
precision balance with 0.001 g readability and the sample was dried by oven at 105ºC. The
samples were conditioned in each climate for 4 days.
Saturated salt solution
Box with tight lid Sample
y [kg/kg]
b
Fan
a
Net
0.113 RH [-] 0.331
Figure 1: Schematic illustration of climate box, and the BET-plot with adsorption isotherm
as a linear function of RH (from [6]).
By plotting the adsorption isotherm (y, see Eq.1) as a function of the RH, the variables a
(interception) and b (slope) were determined by the linear relationship in a BET-plot (see
Figure 1). The specific surface area (SBETH2O) was then calculated according to Eq.2 [1]-[6].
2
Paper III - SCC flowability: Effect of changes in particle
surface area, and how to compensate for this
RH ⋅ mdry
y= [kg/kg] (RH {0;1}) (Eq.1)
( m − mdry ) ⋅ ( 1 − RH )
3.54 ⋅ 10 6
S BETH 2 O = [m2/kg] (Eq.2)
a+b
2.3 Rheology
The rheology was evaluated from the measurements, carried out at 7 and 60 minutes after
adding mixing water, where the sample was let to stand between the runs. The mortar test
measurement was performed using a Bohlin CVO200 rheometer and the concrete a ConTec
Visco5, both using rotating coaxial cylinder at a controlled shear rate ( γ& ) at 20ºC. The
experimental geometry is illustrated in Figure 2. The rheological evaluation of plastic
viscosity (ηpl) and yield stress (σ0) was made according to the Bingham model:
σ = σ 0 + γ& ⋅ η pl [Pa] (Eq. 3).
8 Ro=145 mm Concrete
Ri=100 mm sample
Shear rate [1/s]
4
No logging H=140 mm
2
Logging Rotating
0 outer cylinder
0 10 20 30 40 50 60 Measuring
Time [s] inner cylinder
Figure 2: The experimental setup, and the schematic illustration of the ConTec Visco5
rheometer for concrete (from [6]).
3. BET(H2O)-MODEL
When there is a change in the dry material specific surface area, and as this area has to be
covered with water in order to create mobility, the concrete water demand will change. One
way to compensate for these variations in filler or fine aggregate, is to consider the specific
area by BET(H2O) and translate this to a change in water demand of the concrete mix. With
the assumption that 1 litre of water in one molecule layer covers 3 546 000 m2, the change in
mixing water (∆W) due to a change in specific surface area (∆SBETH2O) can be calculated as:
nH 2O
∆W = ∆S BETH 20 ⋅ ⋅ m mtr [liter/m3] (Eq. 4)
3.546 ⋅ 10 6
where mmtr is the mass of the dry material of the mix, and nH2O is the number of full water
molecular layers covering the particle surfaces required to providing sufficient dispersion for
flowability. Based on numerous experiments, a suitable value was found to be nH2O=30
layers. This can be compared to the proposed, in literature, 5-20 molecular layers of water
adsorbed at high relative humidity [1][4][7][9] or as much as 60 molecular thickness [5].
3
Paper III - SCC flowability: Effect of changes in particle
surface area, and how to compensate for this
100 8 000
L15
80 G100 SBETH2O [m /kg] 6148
6 000
Passing [%]
L40(ref)
2
60 L40
G200 L15
40 4 000
L70 L70
2308
20 G100 1808 1894 1822
2 000
G200
0
0.002 0.004 0.008 0.016 0.032 0.063 0.125 0.25 0.5 0
Size [mm] L40 L15 L70 G100 G200
Figure 3: Size distribution and spec.surface area by BET(H2O) for the five limestone
fillers.
100 4 000
3348
80 3019
2808
SBETH2O [m /kg]
F(ref) 3 000
Passing [%]
2570
G 2341
2
60
H 2 000
40
I
20 J
1 000
Average
0
0.063 0.125 0.25 0.5 1 2 4 8 0
Size [mm] F(ref) G H I J
Figure 4: Size distribution and specific surface area by BET(H2O) for the five “Hol”
gravel.
The concretes were prepared in batches of 40 litres, mixed in a BHS60 twin-shaft paddle
mixer for 4 minutes after water was added to the premixed dry materials.
Two self-compacting mixes were investigated (see Table 2): (1) with the five different
limestone fillers and (2) with the five 0-8 mm natural gravels named “Hol”.
4
Paper III - SCC flowability: Effect of changes in particle
surface area, and how to compensate for this
In order to retain the consistency, relative the mix with the reference material,
complimentary mixes were made with extra water (see Table 3) compensating for the
difference in specific area by BET(H2O). This was made according to Eq. 4.
Table 3: Changes mixing water (∆mw) due to the differences in specific surface area for the
limestone filler and “Hol” gravel.
“Hol”
Limestone ∆SBETH2O ∆mw ∆SBETH2O ∆mw
gravel
filler ID [m2/kg] [kg/m3] [m2/kg] [kg/m3]
ID
L40 (ref) - - F (ref) - -
L15 +499 +0.68 G +229 +1.69
L70 +4 340 +5.89 H +468 +3.45
G100 +86 +0.12 I +679 +5.01
G200 +13 +0.02 J +1007 +7.44
5
Paper III - SCC flowability: Effect of changes in particle
surface area, and how to compensate for this
800
7 min 60 min
600
Spread [mm]
400
200
L40 (ref)
L15 (+0.68)
L70 (+5.89)
G100 (+0.12)
G200 (+0.02)
L15
L70
G100
G200
400 60
507 Pa 7 min 60 min
300
Yield stress [Pa]
Viscosity [Pa s]
7 min 60 min 40
200
20
100
0
0 L40 (ref)
L15 (+0.68)
L70 (+5.89)
G100 (+0.12)
G200 (+0.02)
L15
L70
G100
G200
G100
G200
G100 (+0.12)
G200 (+0.02)
L15
L70
L40 (ref)
L15 (+0.68)
L70 (+5.89)
Figure 5: Flowability measures for the SCC mix with the limestone fillers, both without
and with the extra water added to compensating the BET-surface.
The results from the flowability measures for the mix with the five “Hol” gravel are
presented in Figure 6. Similar to the results for the limestone filler (see Figure 5), the
flowability with the “Hol” gravels shows significant differences between the mixes, which
can be addressed to the differences in BET(H2O)-area. All mixes with extra water achieved
nearly the same consistence as the reference mix with gravel “F”, which indicates that the
differences in surface area can be compensated with water according to the proposed
BET(H2O)-model, see Eq. 4. It can be noted, that thus the gravel size distributions is similar
(see Figure 4), there is up to ~1000 m2/kg difference in BET(H2O)-area. This is ~¼ of the
differences for the limestone filler, but then the content of gravel in the mix is ~4 times
larger then the limestone filler (see Table 2). In [6] it was found that a natural gravel
collected at different spots in a gravel pit, with small differences in grading, can vary in
BET(H2O)-area by ~7000 m2/kg.
6
Paper III - SCC flowability: Effect of changes in particle
surface area, and how to compensate for this
800
7 min 60 min
600
Spread [mm]
400
200
I
H (+3.45)
I (+5.01)
H
G
F (ref)
G (+1.69)
J (+7.44)
J
150 80
60 min 7 min 60 min
60
Yield stress [Pa]
Viscosity [Pa s]
100 7 min
40
50
20
0 0
I
H (+3.45)
I (+5.01)
I
H (+3.45)
I (+5.01)
H
G
F (ref)
G (+1.69)
J (+7.44)
H
G
J
F (ref)
G (+1.69)
J (+7.44)
J
Figure 6: Flowability measures for the SCC mix with the “Hol” gravels, both without and
with the extra water added to compensating the BET-surface.
Question arises whether this extra water added for constant flowability, based on an
increased BET-area, is fixed to the aggregates or fillers and does not contributes to the
concrete hydration. Is it possible to add this extra water without affecting the w/c, in the
same approach made when using the particle water absorption (EN 1097-6 standard)? To
compensate for an increased BET-area by adding extra superplasticizer (SP) to the mix will
not have the same effect as extra water, as the SP (PCE based) normally only reduces the
yield stress and not the viscosity [10]. In Figure 7 the results of the measured compressive
strength for the SCC mix with the different limestone fillers, both without and with the extra
water added to compensating the BET-area, is given. The result shows that the strength is
promoted by increased area, whereas with additional water for constant flowability the effect
is in reverse ratio. This indicates that approx. 50% of this water can be added without
affecting the w/c.
Comp. Strenght, 28d [MPa]
48
No compensation Additional water
47
46
45
L40 L15 L70 G100 G200
Figure 7: Compressive strength (28 days) for the SCC mix with the limestone fillers, both
without and with the extra water added to compensating the BET-area
7
Paper III - SCC flowability: Effect of changes in particle
surface area, and how to compensate for this
6. CONCLUSIONS
An experimental investigation of the effect of the specific surface area of different gravels
and limestone fillers and their influence on the rheology of SCC was carried out. The area
was measured with a simplified BET-method, using water (as moisture) as adsorbate. A
model was presented, where the effect of change in specific area by BET(H2O) is translated
to a change in water demand for constant flowability of the concrete mix. The following
observations and conclusions were made:
Due to the importance of their large surface area, quantification of fillers and the fine
part of aggregates’ properties is essential for the ability to control physical properties,
such as workability, in the production of SCC.
For better quality control and prediction of fresh concrete behaviour, the specific
surface area by BET is proposed as a potential means of geometrical characterization
for fillers and aggregates containing fines.
A coarser material can provide larger surface area than a finer, due to differences in
surface texture and porosity, and thereby negatively influence the flowability.
Addressing to the changes in BET(H2O)-area, a gravel with apparently consistent
grading over time can provide significant differences to the concrete workability.
The proposed model showed that it was possible to calculate the extra water needed to
compensate for changes in filler and fine aggregates BET(H2O)-area, in order to control
and produce SCC with small variations in flowability.
Approximately 30 molecular layers of water, covering the particle surface, are required
to decrease interactions and provide lubrication, sufficient to create flowability.
It was shown that the free water content, available to provide flowability, in 1 m3 SCC
mix can vary by several litres due to differences in apparently equivalent fine
aggregates. A change in BET(H2O)-area of 1000 m2/kg corresponds to approximately
0.8% moisture content of the gravel. E.g. a SCC with 1000 kg gravel (0-8 mm) that
increases by 1 m2/g in area will need 8.5 litre extra water, in order to retain its
consistency.
ACKNOWLEDGEMENTS
Financial support from Färdig Betong and Thomas Concrete Group is greatly appreciated.
REFERENCES
[1] Ahlgren L. (1972): “Moisture fixation in porous building materials”, Division of building
technology the Lund institute of technology, Report 36, Sweden (in Swedish).
[2] Allen T. (1997): “Particle size measurement – Surface area and pore size determination”,
London.
[3] Brunauer S., Emmet H.P., Teller E. (1938): “Adsorption of gasses in multimolecular layers”,
American Chemical Society.
[4] Brunauer S. (1944): “The adsorption of gases and vapours”, vol 1, Oxford.
[5] Eirich F. R. (1960): “Rheology – Theory and applications”, vol 3, New York.
[6] Esping, O. (2004): “Rheology of cementitious materials: effects of geometrical properties of
filler and fine aggregate”, Chalmers University of Technology, Göteborg.
[7] Gregg S. J., Sing K. S. W. (1967): “Adsorption, surface area and porosity”, New York.
[8] Neville A. M. (1963): “Properties of concrete”, London.
[9] Powers T. C. (1968): “The properties of fresh concrete”, New York.
[10] Wallevik O. (2003): “Rheology – A scientific approach to develop self-compacting concrete”,
3rd International Symposium on SCC, Reykjavik.
8
Paper IV - Investigation of autogenous deformation in SCC
Abstract
For modern concretes, such as high-strength and self-compacting concrete (SCC),
increased amount of fines and binder content are a common explanation for the large
autogenous shrinkage and early-age cracking. In order to investigate the influence of
fineness of concrete constituents on autogenous shrinkage, tests with SCC, incorporating
limestone fillers with different specific surface area (by BET), were conducted. A
dilatometer was used, generating measures of linear autogenous (sealed) deformation of the
concrete cast in vapour-proof flexible tube mould. Temperature and pore pressure were
simultaneously measured with the deformation. Tests were conducted on mixes both with
and without cement, i.e. with and without chemical shrinkage. The results indicated that
increased surface area generated an increased magnitude and rate of autogenous shrinkage,
without influencing the times to initial and final set. The mixes without cement appeared to
generate a large “autogenous” shrinkage, without the presence of chemical reaction of
cement and water (hydration). The shrinkage was approximately 0.8 mm/m at 24 hours, after
an initial swelling up to 4 hours. This is the same magnitude as for the mixes with cement,
but then these mixes generated no swelling and almost all shrinkage before final set (at ~11.5
hours from mixing). Increased particle surface area also decreased the rate and magnitude of
evaporation, and consequently reduced the plastic crack tendency, despite increased
autogenous shrinkage. Adding extra water to the mix, compensating for the loss of
flowability due to increased particle surface area, increased the crack tendency significantly.
INTRODUCTION
Early-age shrinkage and cracking have become a recurrent problem in concrete
construction. Conditions such as reduced maximum aggregate size, increased amount of
fines, presence of retarding admixtures, increased binder content, and deficient covering and
curing all contribute to this problem.
At early age, when the cement paste is young and has poorly developed mechanical
properties, autogenous and drying shrinkage, both incorporated in the plastic shrinkage, are
the two main driving forces for cracking. When the concrete dries out due to evaporation, the
loss of water from the paste generates negative capillary pressure, causing the paste to
contract (see Wittmann [1]), which in turn can lead to cracks. These contracting capillary
forces are in reverse ratio to the meniscus radius, and hence the capillary tension stresses
increase with decreasing pore sizes and interparticle spaces. Care has to be taken to protect
the surface against drying, although experience in the use of concretes with low w/b has
revealed that severe cracking may occur in spite of proper protection (curing membrane,
1
Paper IV - Investigation of autogenous deformation in SCC
etc.); see Bjøntegaard et al. [2]. For a concrete where evaporation is prevented, a contracting
negative capillary pressure will also develop, but only once the hydration commences and
the concrete sets (see Holt [3]). As long as the concrete is fluid, autogenous shrinkage is
considered to be equal to the chemical shrinkage; but once the self-supporting skeleton starts
to form, the autogenous will diverge from the chemical (e.g. Hammer [4], Jensen & Hansen
[5]). The pattern of autogenous deformation, exemplified in Figure 1, comprises three
distinct stages which can be defined as (I) plastic, (II) semiplastic and (III) rigid, separated
by the time to initial and final set; see Esping & Löfgren [6]. It has been suggested (e.g. by
Barcelo [7]) that, when measuring the autogenous deformation, the setting will be
manifested as a change of the slope of the deformation. Furthermore, once the internal voids
are created, it leads to the development of a capillary pore underpressure in the skeletal
structure (see Figure 1), which causes an external deformation of the hardening concrete (see
Radocea [8]).
Water
Deformation, Pressure & Temp
It can be argued that the deformation occurring when the concrete is plastic mainly causes
setting and has little consequence for the risk of cracking, while the shrinkage taking place
when the concrete is semiplastic is considerably more detrimental as the concrete at this
stage has poorly developed tensile strain capacity; see Kasai et al. [9].
This paper aims at demonstrating how changes in particle specific surface area affect the
early-age deformations, primarily the autogenous.
In this study, the change in area is represented by limestone fillers with different specific
surface area quantified with the BET(H2O) method. Furthermore, early age is considered as
the time from mixing up to 24 hours after mixing. The term ‘deformation’ is preferably used,
since expansion also may occur. Autogenous deformation is considered to be the bulk
deformation under sealed conditions, and is referred to the full period of hardening from the
time when water was added to the mix. Linear displacement was used for measuring
autogenous deformation. No corrections were made for the differences between linear and
volumetric changes during the fluid state (before initial set). Moreover, ideal isothermal
conditions are attributed to autogenous deformation, and this was not strictly the case. No
compensation for thermal changes was made.
2
Paper IV - Investigation of autogenous deformation in SCC
TEST METHODS
0%
Length change (deformation)
y = 0,338x
Specimen length 400 mm -1%
Adjustable Digital gauge
fixture Mould diameter 82 mm (1/1000 mm)
-2% y = 0,796x
2
y=x R = 0,9999
0 001
-3%
3-D tube (calculated)
-4% Fluid (measured)
1-D tube (calculated)
-5%
0% -1% -2% -3% -4% -5%
Volume change
Figure 2: To the left, illustration of the Concrete Digital Dilatometer (CDD) for linear
autogenous deformation measurement (from Esping & Löfgren [6]). To the right,
the ratio between linear and volumetric deformation for the mould. Filled with a
Newtonian fluid the ratio follows the measured ratio, but once rigid the ratio will
follow the calculated 3-D deformation (from [12]).
3
Paper IV - Investigation of autogenous deformation in SCC
100 8 000
Specific surface area, BET(H2O) [m /kg]
2
6150
80
6 000
Passing [%
60
4 000
L40
40
L15
2310
L70 1810 1890 1820
2 000
20 G100
G200
0 0
0.002 0.004 0.008 0.016 0.031 0.063 0.125 0.25 0.5 L40 L15 L70 G100 G200
Size [mm]
Figure 3: The five limestone fillers. To the left is the size distribution, and to the right the
specific surface area measured with the BET(H2O) method.
Mixes were also made without presence of cement, in order to evaluate the effect (if any)
of particle surface area on the autogenous deformation without influence of chemical
shrinkage. The cement was replaced with an equal volume of limestone filler, i.e. the filler
content was increased from 160 to 458 kg/m3. Concrete flowability strongly depends on the
size of the particle surface area which has to be covered with water to create mobility. When
the specific surface area increases, so will the water demand of the mix for the same
consistency. Using L40 as reference, extra water was added to the mixes, compensating for
the differences in surface area by BET(H2O) and regaining constant flowability. A model
was used where 30 molecular layers of water covering the particle surface are required to
decrease interactions and provide lubrication sufficient to create flowability; see Esping [15].
4
Paper IV - Investigation of autogenous deformation in SCC
In Table 2 the changes in recipe, due to differences in specific area of limestone filler, are
given. This was only applied to the plastic shrinkage ring test, as the effect of water content
on autogenous deformation has previously been demonstrated by Esping & Löfgren [12].
Table 2: Mixing water with compensations for the differences in specific surface area of
limestone fillers. L40 is used as reference (smallest surface area).
ID L40 (ref) L15 L70 G100 G200
3 187.02 (+0.02)
W 187 liter/m 187.68 (+0.68) 192.89 (+5.89) 187.12 (+0.12)
RESULTS
0 100
L40
Rate of deformation [10 /h]
-6
Deformation [10 m/m]
G200 0
-300
G100
-6
L15 -100
L40
-600
G200
-200
G100
-900 L15
-300
L70 L70
-1200 -400
0 6 12 18 24 0 6 12 18 24
Time (from mix) [hour] Time (from mix) [hour]
(a) (b)
Figure 4: SCC w/c 0.55 containing limestone filler with different specific area: (a) the
autogenous deformation and (b) the rate of deformation.
5
Paper IV - Investigation of autogenous deformation in SCC
-400 15
Rate of deformation [10 /hour]
-300
Semiplastic 10
-200
5
-100 Initial set
Final set
0 0
L40
L15
L70
G100
G200
L40
L15
L70
G100
G200
(a) (b)
Figure 5: Evaluated values from autogenous deformation in the plastic and semiplastic
period: (a) the rate of autogenous deformation and (b) the rate of deformation.
Furthermore, Figure 6(a) shows the development of pore pressure, and Figure 6(b) the
evaluated maximum rate of pore pressure which occurred at approximately 7-8 hours from
mixing. The time to and magnitude of maximum underpressure could not be evaluated due
to the loss of pressure at random times. This effect is usually referred to as the breakthrough
pressure; see Wittman [1].
0 -60
G200
-20
Pore pressure [kPa]
dP/dt [kPa/hour]
-40
-40
L40
-60
L70
-20
-80 G100
L15
-100
0 3 6 9 12 0
Time (from mix) [hour] L40 L15 L70 G100 G200
(a) (b)
Figure 6: SCC w/c 0.55 containing limestone filler with different specific area: (a) the
development of capillary pore pressure during the first 12 hours from mix, and
(b) the maximum rate of pore pressure (at approximately 7-8 hours from mix).
6
Paper IV - Investigation of autogenous deformation in SCC
Temp. Temp.
Temp.
Pore
Pore Pore
pressure
pressure pressure
Autogenous Autogenous
Autogenous
deformation deformation
deformation
Min
0 5 10 15 20 0 5 10 15 20 0 5 10 15 20
Time (from mix) [hour] Time (from mix) [hour] Time (from mix) [hour]
Pore Pore
pressure pressure
Autogenous
Autogenous
deformation
deformation
Min
0 5 10 15 20 0 5 10 15 20
Time (from mix) [hour] Time (from mix) [hour]
7
Paper IV - Investigation of autogenous deformation in SCC
800 600
L15
400 400
L70 L40
-6
L15
0 L40 200 G100
G100 G200
G200
0
-400
-200
-800 0 6 12 18 24
0 6 12 18 24 Time (from mix) [hour]
Time (from mix) [hour]
(a) (b)
Figure 8: The mix without cement (same composition as SCC w/c 0.55, but cement is
replaced with equal-volume limestone filler): (a) the “autogenous” deformation
and (b) the rate of deformation.
Max 80
No compensation
Average crack area [mm ]
2
60 Extra water
Pore pressure (low)
Pore pressure (high)
40
Evaporation
Temperature
Strain 20
Initial crack
Min
0
0 5 10 15 20
L40(ref) L15 L70 G100 G200
Time (from mix) [hour]
(a) (b)
Figure 9: In (a) is the development of pore pressure, evaporation, temperature and strain
(normalized against maximum values), exemplified by the concrete with
limestone filler L40. In (b) is the crack tendency for the respective filler without,
and with, extra water compensating for the differences in surface area.
When adding extra water to compensate for the loss in flowability, the crack tendency
increased significantly. The differences in crack tendency are most likely a consequence
mainly of evaporation, which is verified by the measured evaporation in Figure 10(a) and its
8
Paper IV - Investigation of autogenous deformation in SCC
initial rate (up to 4 hours from mix, before initial setting) in Figure 10(b). A large particle
surface area lowers the evaporation, whereas extra water increases the evaporation.
3 0,5
L70(+5,87)
No compensation
Extra water
2
2
2
L15
L70
L40(ref) 0,4
G100
1 G100(+0.12)
G200
G200(+0.02)
0
0,3
0 5 10 15 20
L40(ref) L15 L70 G100 G200
Time (from mix) [hour]
(a) (b)
Figure 10: SCC w/c 0.55 containing limestone filler with different surface area and extra
water compensating for this: (a) the measured evaporation and (b) the evaluated
initial rate (<4 hours from mix).
CONCLUSIONS
An experimental investigation of early-age (<24 hours) deformation was made on a series
of self-compacting concretes with w/c 0.55 containing limestone filler with different specific
surface area measured with BET(H2O). Autogenous linear deformations were measured and
additional investigation of plastic crack tendency was carried out, both complemented by
simultaneous measurements of pore pressure and temperature development.
9
Paper IV - Investigation of autogenous deformation in SCC
ACKNOWLEDGEMENTS
Financial support from AB Färdig Betong is greatly appreciated.
REFERENCES
[1] Wittmann, F.H., ‘On the Action of Capillary Pressure in Fresh Concrete’, Cement and Concrete
Research, Vol. 6, pp. 49-56, 1976.
[2] Bjøntegaard Ø., Hammer T. A., Sellevold E. J., ‘Cracking in High Performance Concrete before
Setting’, Symposium on High-Performance and Reactive Powder Concretes, Sherbrooke, 1998.
[3] Holt, E. E., ‘Early age autogenous shrinkage of concrete’. Technical Research Centre of Finland,
VTT Publication 446, Finland, 2001.
[4] Hammer T. A., ‘Test method for linear measurements of autogenous shrinkage before setting’, in
Autogenous shrinkage of concrete (ed. Tazawa E.), E & FN Spon, London, pp. 143-154, 1998.
[5] Jensen O. M., Hansen F., ‘Autogenous deformation and RH-change in perspective’, Cement and
Concrete Research, Vol. 31, pp. 1859-1865, 2001.
[6] Esping, O., Löfgren, I., ‘Cracking due to plastic and autogenous shrinkage – Investigation of
early age deformation of self-compacting concrete’, Publication 05:11, Chalmers, Sweden, 2005.
[7] Barcelo, L., Moranville, M., and Clavaud, B., ‘Autogenous shrinkage of concrete: a balance
between autogenous swelling and self-desiccation’, Cement and Concrete Research, Vol. 35, pp.
177-183, 2005.
[8] Radocea A., ‘A Study on the Mechanisms of Plastic Shrinkage of Cement-Based Materials’,
Doctoral dissertation, Chalmers, Sweden, 1992.
[9] Kasai, Y., Yokoyama, K., and Matsui, I., ‘Tensile Properties of Early Age Concrete’,
Mechanical Behavior of Materials, Society of Materials Science, Vol. 4, pp. 288-299, Japan,
1972.
[10] Jensen O. M., Hansen F., ‘A dilatometer for measuring autogenous deformation in hardening
Portland cement paste’, Materials and Structures, Vol. 28 (181), pp. 406-409, 1995.
[11] Aïctin, P.C., ‘Autogenous shrinkage measurement’, in Autogenous shrinkage of concrete (ed.
Tazawa E.), E & FN Spon, pp. 257-268, 1999.
[12] Esping, O., Löfgren, I., ‘Investigation of early age deformation in self-compacting concrete’,
Conference advanced cement-based materials, DTU, Denmark, 2005.
[13] Johansen, R., Dahl, P.A., ‘Control of plastic shrinkage of cement’. 18th Conference on Our
World in Concrete and Structures, Singapore, 1993.
[14] Löfgren, I., Esping, O., ‘Early age cracking of self-compacting concrete’, RILEM Conference of
Volume Changes of Hardening Concrete, Denmark, August 2006.
[15] Esping O., ‘Rheology of cementitious materials – Effects of geometrical properties of filler and
fine aggregate’, Licentiate thesis, Publication No. P-04:3, Chalmers, Sweden, 2004.
[16] Nawa T., Horita T., ‘Autogenous shrinkage of high-performance concrete’, Proceedings on
microstructure and durability to predict service life of concrete structures, Japan, 2004.
[17] Hammer T. A., ‘Is there a relationship between pore water pressure and autogenous shrinkage.
Before and During Setting?’, in Self-desiccation and its importance in concrete technology,
Lund University of Technology, TVBM-3104, pp. 27-38, 2002.
10
Paper V - Investigation of early age deformation in SCC
Abstract
In the presented work, early age (< 24 h) autogenous deformation was measured and
crack tendency due to plastic shrinkage was evaluated; see Esping and Löfgren [1]. For the
autogenous deformation, a specially developed digital dilatometer was used which generated
accurate measurements of the linear displacements of the concrete, which was cast in a
vapour-proof flexible tube mould. The plastic shrinkage cracking tendency was evaluated by
exposing concrete specimens to early drying conditions while these were restrained by an
inner steel ring. A large number of different SCC constituents and mix compositions have
been investigated: e.g. w/c-ratio from 0.38 to 0.67, silica fume, and different admixtures. For
comparison, tests with standard concrete were also made. The influence of different
constituents and mixes on the autogenous deformation and plastic shrinkage crack tendency
was observed. The results indicated that a high crack tendency arose when there was: large
autogenous shrinkage (silica addition, low w/c, high fineness); high water evaporation (high
w/c, low fineness); retardation (retarder or high superplasticizer dosage); low content of
coarse aggregate. Minimum crack tendency was found at w/c 0.55.
1. INTRODUCTION
At early age, when the cement paste is young and has poorly developed mechanical
properties, autogenous and drying shrinkage – both incorporated in the plastic shrinkage –
are the two main driving forces for cracking. Generally, plastic shrinkage is usually defined
as the shrinkage of fresh concrete, exposed to drying, that takes place during the time when
the concrete is ‘plastic’, the duration is usually short (< 8 to 12 hours) and ends when the
concrete has reached its final set. In traditional concretes plastic shrinkage cracking is mainly
caused by the loss of water from the fresh concrete, e.g. by evaporation of water, which
generates negative capillary pressures; this cause the paste to contract (see Wittmann [2]),
which in turn can lead to cracks. These contracting capillary forces are in reverse ratio to the
meniscus radius, and hence the capillary tension stresses increase with decreasing
interparticle spaces. For a concrete where evaporation is prevented, a negative capillary
pressure will also develop, but only once the hydration commences and the concrete sets. To
avoid this type of cracks, care has to be taken to protect the surface against drying. However,
experience in the use of concretes with low w/b has revealed that severe cracking may occur
in spite of proper protection (curing membrane, etc). Conditions such as reduced maximum
aggregate size, presence of retarding admixtures, increased binder content, and deficient
curing all contribute to this problem. Early cracking is usually observed in the period soon
1
Paper V - Investigation of early age deformation in SCC
after casting up to 6-8 hours later, depending on the concrete temperature, material
composition, weather conditions and the degree of retardation. In this early phase, the
rheology of concrete changes dramatically as the concrete sets, i.e. it changes from a liquid
to a solid behaviour within some hours. At the same time the tensile strain capacity goes
through a minimum. The cause of this change in rheology is the hydration of Portland
cement, which is a complex sequence of chemical reactions leading to setting and hardening.
Immediately after mixing cement and water, reactions start to occur and these generate an
outburst of heat (Stages I in Figure 1). After these initial stages an induction period, or
dormant period, is entered (Stage II). During the induction period not much hydration takes
place, but this does not mean that the paste is ‘dormant’ with respect to volume changes.
Setting (during Stage III) is defined as the onset of rigidity in fresh concrete, and the
period of fluidity, preceding setting, corresponds to the induction period (Stage II); see
Figure 1(a). As long as the concrete is fluid, there will be a linear relationship between the
linear shrinkage and the volumetric chemical shrinkage. However, once the self-supporting
skeleton starts to form, the chemical shrinkage will mainly result in internal voids and the
linear deformation diverges from the chemical shrinkage. It has been suggested (e.g. by
Barcelo [4]) that, when measuring the linear deformation, the setting will be manifested as a
change of the slope of the deformation; see Figure 1(b). Furthermore, once the internal voids
are created it leads to the development of a capillary underpressure in the skeletal structure,
see Figure 1(b), which causes an external deformation of the hardening concrete. It can be
argued that the deformation occurring when the concrete is plastic may have little
consequence for the risk of cracking, while the shrinkage taking place when the concrete is
semiplastic is considerably more detrimental as the concrete at this stage has poorly
developed mechanical properties (low tensile strength and strain capacity).
Dissolution: Plastic Semiplastic Rigid
Deformation, Pressure & Temperature
reactions Temperature
Rapid formation Pressure
of C-S-H and CH
Formation of
Induction period: monosulfate
increase in Ca2+
concentration Final set
Initial set
Initial set Deformation
I II III IV V
0 ~6 ~12 ~18 ~24
~10 m ~4 h ~12 h ~24 h Time (from mixing) [hour]
Time of hydration I & II III & IV V
(a) (b)
Figure 1: (a) Heat evolution during hydration (based on [3]) and (b) early-age linear
autogenous deformation of concrete and the corresponding development of
temperature and capillary pore pressure (from [1]).
2. TEST METHODS
2
Paper V - Investigation of early age deformation in SCC
with a pair of hose clamps and 30 mm thick PVC end-caps equipped with O-ring sealing.
The mould was placed in a mechanical stable measuring rig, where a digital gauge recorded
the unrestrained linear deformation with an accuracy of 0.003 mm. The test was performed
in a thermostable room at 20ºC, where the measurement recording was started at 30 minutes
from water addition. The equipment and apparatus for a typical test are shown in Figure 2,
and for each test three complete CDD set-ups were used. The experiments have also been
supplemented with measurements of temperature and pore pressure in sealed specimens.
Specimen length 400 mm Didital gauge
Adjustable Mould diameter 82 mm 1/1000 mm
fixture
0 001
0 001
Figure 2: Test arrangement of the Concrete Digital Dilatometer (CDD) for linear
autogenous deformation measurement (from [1]).
Fan
Climat conditions:
Average crack area =
∑ (crack length × crack width )
23±2 ºC
3
35±5% RH
Air funnel
Air velocity Steel rings
4.5 m/s
(Ø300/600)
Sample
10 Sample
80
Stress raisers
Scale Base plate
Ø 300
(steel)
Ø 600
Figure 3: Test arrangement for the determination of the cracking tendency (from [1]).
3
Paper V - Investigation of early age deformation in SCC
3. EXPERIMENTAL PROGRAM
3.1 Materials
The mix design and its constituents, as used in this study, comprise typical materials and
compositions for self-compacting concrete (SCC) in Sweden. The properties of the dry
materials and admixtures are listed in Table 1 and Table 2. The concretes were prepared in
batches of 40 or 60 liters, mixed in a twin-shaft paddle mixer for 4 minutes after water was
added to the premixed dry materials. The admixtures were added directly after the water.
In order to evaluate the effect of constituent type and dosage, a number of different mixes
were investigated. The following mixes are presented in this paper (for the full experimental
study see [1]):
1. Reference concretes: w/c 0.38, 0.45, 0.55 and 0.67 (see Table 3).
2. Silica fume: 5% and 10% SF by cement weight (SF replaced equal C volume).
3. Coarse aggregate content: 20%, 30%, 40% (REF) and 50% A 8-16 of total volume of
aggregate. The changes were replaced by equal volume of A 0-8.
4. Superplasticizer dosage: 0.6%, 0.8% (REF) and 1.0% SP dosage of C weight.
5. Accelerator and retarder: 1.5% ACC and 0.2% RE by C weight.
6. Shrinkage-reducing admixture: 1.0% and 2.0% SRA by C weight.
7. Conventional concrete: w/c 0.55 with 345 kg cement and 60/40% (0-8 mm/8-16 mm)
aggregate; and w/c 0.67 with 330 kg cement and 60/40% (0-8 mm/8-16 mm) aggregate.
4
Paper V - Investigation of early age deformation in SCC
4. RESULTS
-6
-400 -25
-6
(a) (b)
Figure 4: Autogenous deformation of self-compacting concrete with w/c from 0.38 to 0.67
(a) and (b) rate of deformation (from [1]).
5
Paper V - Investigation of early age deformation in SCC
Pressure & Deformation [-] Pressure w/c 0.45 Pressure w/c 0.67
Temperature [-]
Temperature [-]
Temp.
Temp.
Final set
Final set
Deformation
Initial set
Deformation
0 5 10 15 20 0 5 10 15 20
Time [hours] Time [hours]
(a) (b)
Figure 5: Development of temperature, capillary pore pressure, and autogenous
deformation (the axes have been normalized against maximum values): (a) for
concrete with w/c 0.45; and (b) for concrete with w/c 0.67 (from [1]).
It is well known that silica fume increases the autogenous shrinkage, as well as
accelerating the early hydratation and initiating the stiffness at earlier age. The results of the
autogenous deformation measurements for the concretes with silica fume are presented in
Figure 6. These results indicate that addition of silica fume increased the magnitude and rate
of autogenous shrinkage in all periods (in the plastic, semiplastic, and rigid periods), and the
effect increased with increased silica dosage. Silica fume decreased the plastic time period,
and the effect increased with increased silica dosage. No changes in semiplastic time could
be observed.
0 6 12 18 24 0 6 12 18 24
Rate of deformation [10 m/m/hour]
0 25
-200 0
Deformation [10 m/m]
-400 -25
-6
-600 -50
w/c 0.55 (ref)
-800 w/c 0.55 Si 5% -75
w/c 0.55 Si 5%
w/c 0.55 Si 10%
-1 000 -100
w/c 0.55 Si 10%
-1 200 -125
Time [hours] Time [hours]
(a) (b)
Figure 6: Effects of silica fume (Si) on: (a) the autogenous deformation of self-compacting
concrete with w/c from 0.55 and (b) the rate of deformation (from [1]).
The results for the concrete with varying coarse aggregate content are presented in Figure
7. It should be noted that the content of coarse aggregate had a large impact on the rheology,
which can be deduced from the aggregate packing. Good packing improves the flowability
as more water is made available for dispersing the particles. The results indicate that
increased coarse aggregate content decreased both the magnitude and rate of autogenous
6
Paper V - Investigation of early age deformation in SCC
deformation. The effect was more apparent at higher content of coarse aggregate, which
might be explained by the coarser particles’ ability to create a restraining matrix. No
significant changes in times for the plastic and semiplastic periods could be observed, but an
increased content of coarse aggregate tended to delay the rigid period.
0 6 12 18 24 0 6 12 18 24
0
-6
-200
-6
-25
w/c 0.55 30% (8-16)
-50
w/c 0.55 20% (8-16)
w/c 0.55 50% (8-16)
-400 -75
w/c 0.55 (ref) 40% (8-16)
-100 w/c 0.55 30% (8-16)
w/c 0.55 20% (8-16)
-600 -125
Time [hours] (w/c 0.55) Time [hours]
(a) (b)
Figure 7: Effects of coarse aggregate content (8-16) on: (a) the autogenous deformation
and (b) the rate of deformation (from [1]).
The results of the autogenous deformation measurements for the concrete with shrinkage
reducing admixture (SRA) are presented in Figure 8. The results indicate that addition of
SRA decreased the magnitude and rate of autogenous shrinkage for all concretes, and the
effect increased with increased SRA dosage. In the semiplastic period the effect of SRA was
not as pronounced as in the plastic and rigid periods. SRA showed no effect on the times of
the plastic and semiplastic periods.
0 6 12 18 24 0 6 12 18 24 0 6 12 18 24
0
-800
Time [hours] Time [hours] Time [hours]
It is well known that SP retards the concrete, as it delays the early hydration and initiates
the stiffness at higher age. The results of the autogenous deformation measurements clearly
7
Paper V - Investigation of early age deformation in SCC
verify these phenomena, as can be seen in Figure 9(a). The results indicate that with
increased SP dosage the magnitude of autogenous shrinkage increased, which can be
explained by improved cement dispersion; see Holt [8]. An increased SP dosage also
increased the rate of shrinkage in the plastic and semiplastic periods. After setting, the effect
was the opposite, where the rate of shrinkage decreased with SP dosage. Moreover, an
increased SP dosage prolonged the plastic time period, while no changes in the semiplastic
time could be observed.
The results of the autogenous deformation measurements for the concrete with accelerator
(ACC) and retarder (RE) are presented in Figure 9(b). The results indicate that in the plastic
period (before initial setting), the accelerator increased the magnitude and rate of shrinkage
while the retarder hade the opposite effect, which could be expected. In the semiplastic
period, the accelerator and retarder showed no significant effect on magnitude and rate of
shrinkage. In the rigid period, both the accelerator and retarder increased the rate of
shrinkage. The accelerator tended to shorten the time to initial setting while the retarder
tended to delay it. According to the supplier (SIKA), RE will have a small delaying effect at
early hydration (to initial setting), and ACC will have no effect in the same period. The
results in this study showed the same tendency.
0 6 12 18 24 0 6 12 18 24
0 0
w/c 0.67 SP 0.6%
w/c 0.67 ACC (1.5%)
Deformation [10 m/m]
-6
-400 -400
(a) (b)
Figure 9: Autogenous deformation of concrete with w/c 0.67: (a) effect of superplasticizer
dosage (SP) 0.6%, 0.8%, and 1.0%; and (b) effect of accelerator (ACC) and
retarder (RE) (from [1]).
8
Paper V - Investigation of early age deformation in SCC
0.37 and 0.44 kg/m2/h (the low values for w/c ≤ 0.45); this can be compared with the
evaporation from a free water surface of 0.50 kg/m2/h under same conditions.
150 4
conv. w/c 0.67
conv. w/c 0.55
Average crack area [mm ]
2
Conventional Water
3
Evaporation [kg/m ]
2
100
SCC SCC w/c 0.67
2
When silica fume replaced 5% and 10% of the cement in the concrete with w/c 0.55, the
average crack area, which can be seen in Figure 11(a), increased dramatically. The effect
that silica fume had on the evaporation can be seen in Figure 11(b). Silica reduced the
evaporation. A possible explanation for the increased crack area is an increased amount of
small particles, which increased the autogenous shrinkage, as could be seen in the CDD
experiments.
150 4
Average crack area [mm ]
2
3
2
100
2
w/c 0.55 Si 5%
50
w/c 0.55 1 w/c 0.55 Si 10%
0 0
0% 5% 10% 0 6 12 18 24
Silica [weight% of Cement] Time [hours]
(a) (b)
Figure 11: Influence of silica fume (Si) on: (a) the crack susceptibility and (b) the
evaporation (from [1]).
That the aggregates are important is well known, and it is beneficial to have large
aggregates and a high aggregate content. The effect of the coarse aggregate content (8-16 in
relation to total aggregate content) on crack area can be seen in Figure 12(a). As the coarse
aggregate was reduced, the crack area increased. Interestingly, however, an increased
amount of fine aggregate content also reduced the evaporation, as can be seen in Figure
12(b). This indicates that it is not only the evaporation which determines the cracking
behaviour; also the autogenous deformation plays an important role.
9
Paper V - Investigation of early age deformation in SCC
50 4
40
3
Evaporation [kg/m ]
2
w/c 0.55
30
2
20
w/c 0.55 30% 8-16
10 1
0 0
30% 40% (ref) 0 6 12 18 24
Coarse agg. content [vol% of total] Time [hours]
(a) (b)
Figure 12: Influence of coarse aggregate content (8-16) on: (a) the crack susceptibility and
(b) the evaporation (from [1]).
The shrinkage-reducing admixture (SRA) had a positive effect on the crack area. As can be
seen in Figure 13(a), for both the investigated concretes (w/c 0.55 and 0.67) the crack area
was reduced with SRA. The effect of SRA on the evaporation can be seen in Figure 13(b).
This effect starts to be notable at about three hours, after which point the evaporation and its
rate were significantly lower for the concretes containing SRA. The main effect of the SRA
is that it reduces the surface tension of the water (or pore solution), which has a positive
effect on shrinkage as it reduces the capillary tension caused by a reduction in pore radius.
However, the SRA also influences the rate of drying; the concretes containing SRA had a
significantly lower weight reduction than the reference concretes, and the mechanism is
notable as soon as the hydration starts.
100 4
w/c 0.67 (ref)
Average crack area [mm ]
2
3
2
w/c 0.67
60
2
40
w/c 0.55 SRA 2%
w/c 0.55
1 w/c 0.67 SRA 1%
20
w/c 0.67 SRA 2%
0 0
0% 1% 2% 0 6 12 18 24
Shrinkage reducer [weight% of Cement] Time [hour]
(a) (b)
Figure 13: Influence of shrinkage-reducing admixture (SRA) on: (a) the crack susceptibility
and (b) the evaporation (from [1]).
The superplasticizer dosage seemed to have a large influence on the average crack area.
As can be seen in Figure 14(a), when the SP-dosage was reduced to 0.6% the crack area was
significantly reduced, and with the high SP-dosage (1.0%) the crack area increased. For the
case with a delayed additional SP-dosage (0.2% after 30 min) the crack area increased even
10
Paper V - Investigation of early age deformation in SCC
more. The effect that the superplasticizer (SP) dosage had on the evaporation is presented in
Figure 14(b). An increased dosage, as in the case with 1.0% and with a delayed dosage of
0.2%, resulted in an increased evaporation. With a reduced SP-dosage, 0.6%, the evaporation
was reduced. That the evaporation increases is probably a result of the prolonged setting
time.
200 4
w/c 0.67 SP 0.8% + w/c 0.67 SP 0.8+0.2%
Average crack area [mm ]
2
Evaporation [kg/m ]
150 3
2
100 2
w/c 0.67 (ref)
SP 0.8%
50 1
w/c 0.67 w/c 0.67 SP 0.6%
0 0
0,6% 0.8% (ref) 1,0% 0 6 12 18 24
SP dosage [weight% of Cement] Time [hours]
(a) (b)
Figure 14: Influence of superplasticizer (SP) dosage on: (a) the crack susceptibility and (b)
the evaporation (from [1]).
Similarly to the effect of the SP-dosage, accelerating and retarding the concrete had a
considerable effect on the crack area, as can be seen in Figure 15(a). For the concrete with
accelerator the crack area was reduced, while for the concrete with retarder the crack area
increased. The effect that the accelerator and the retarder had on the evaporation can be seen
in Figure 15(b), and is comparable to the effect that the SP-dosage had. For the concrete with
accelerator the evaporation was reduced, and for the concrete with retarder the evaporation
increased.
150 4
w/c 0.67 RE (0.2%)
Average crack area [mm ]
2
w/c 0.67
Evaporation [kg/m ]
3
2
100
2
w/c 0.67 (ref)
50
w/c 0.67 ACC (1.5%)
1
0 0
ACC (1.5%) Reference RE (0.2%) 0 6 12 18 24
SP dosage [weight% of Cement] Time [hours]
(a) (b)
Figure 15: Influence of accelerator (ACC) and retarder (RE) on: (a) the crack susceptibility
and (b) the evaporation (from [1]).
11
Paper V - Investigation of early age deformation in SCC
5. DISCUSSION
Based on the results of this study, the following paragraph contains a general discussion
of the mechanisms leading to the formation of plastic shrinkage cracks, and a brief
description of possible actions to counteract them is presented. The formation of plastic
shrinkage cracks is governed by the development of capillary pore pressure. However,
depending on the characteristics of the concrete, different mechanisms are responsible. For
concrete with a high w/c-ratio, evaporation is the governing mechanism, while for concrete
with a low w/c-ratio (or with the addition of silica) the autogenous deformation is the driving
force. This is presented in Figure 16, which also indicates that the optimum concrete has a
w/c-ratio of 0.55. These observations also suggest that, in order to avoid plastic shrinkage
cracking, different actions need to be taken depending on the type of mechanism. A concrete
with a high w/c needs to be protected against early evaporation (e.g. by a curing membrane:
see [1]). For a concrete with a low w/c-ratio, protection against evaporation may not help, as
experience shows (see [9]), and the autogenous deformation needs to be reduced. This can be
achieved for example with a shrinkage-reducing admixture (which also reduces evaporation)
or by an increased coarse aggregate content.
6
Relative crack area [-]
0 6 12 18 24 4
0 2 Water w/c 0.67
Evaporation [kg/m ]
2
w/c 0.67
Deformation [10 m/m]
3
w/c 0.55
-6
-400 0 2
0.38 0.45 0.55 0.61 0.67
w/c 0.55
w/c 1
-800 w/c 0.45
w/c 0.45 w/c 0.38
w/c 0.38 w/c < 0.55 w/c > 0.55 0
-1 200 Autogenous w/c 0.55 Evaporation 0 6 12 18 24
Time [hours] deformation optimal Time [hours]
Figure 16: Separation of mechanisms governing the formation of plastic shrinkage cracks.
6. CONCLUSIONS
An experimental investigation of early age deformation and cracking tendency was made
on a number of self-compacting concretes, having w/c-ratio between 0.38 and 0.67, and the
influence of various mix parameters was investigated. Autogenous deformations were
measured and the cracking tendencies were investigated in a restraint ring specimen.
The results from the measurements of linear autogenous deformation by the CDD show that:
− Increased cement content (lower w/c) increased the rate of and total chemical
shrinkage and thereby the autogenous deformation.
− Increased coarse aggregate content decreased the magnitude and rate of autogenous
deformation.
− Addition of silica fume increased the magnitude and rate of autogenous shrinkage and
the effect increased with increased silica dosage. Silica fume decreased the time of the
plastic period.
12
Paper V - Investigation of early age deformation in SCC
The conclusions that can be drawn from the restraint ring tests are that:
− The rate of evaporation was not always the governing factor for the cracking tendency.
− Silica fume led to increased autogenous deformation (the CDD experiments) and
increased crack area in the ring test, though the evaporation was reduced.
− Reduced aggregate content increased autogenous deformation, while the evaporation
was reduced.
− A shrinkage-reducing admixture (SRA) proved to be very effective in reducing the
cracking tendency. SRA reduced the autogenous deformation as well as the
evaporation.
− Delaying/retarding the hydration, with increased SP-dosage or by adding a retarder,
increased both the autogenous deformation (the CDD experiments) and the crack area.
− Accelerating the hydration, e.g. by adding an accelerator, decreased both the
autogenous deformation (the CDD experiments) and the crack area.
− The concrete with the high w/c-ratio (0.67) had the highest crack area. Furthermore,
there seems to exist an optimum w/c-ratio for the investigated mixes, which indicates
that the w/c-ratio should be in the region of 0.55; see Figure 10(a).
− The conventional concrete showed a similar tendency as the SCC (minimum cracking
tendency at w/c 0.55) but, due to higher evaporation, it was found to be more
susceptibile to cracking.
ACKNOWLEDGEMENTS
Financial support from SBUF (the Swedish construction industry’s organisation for
research and development) and AB Färdig Betong is greatly appreciated.
REFERENCES
[1] Esping, O. and Löfgren, I., 'Cracking due to plastic and autogenous shrinkage – Investigation of
early age deformation of self-compacting concrete – Experimental study', Publication No 05:11,
Department of Building Technology, Chalmers University of Technology, Göteborg 2005, 95
pp.
[2] Wittmann, F.H., 'On the Action of Capillary Pressure in Fresh Concrete', Cement and Concrete
Research, Vol. 6 (1976), pp. 49–56.
[3] Gartner, E.M., Young, J.F., Damidot, D.A., and Jawed, I., 'Hydration of Portland cement'.
Chapter 3 in Structure and performance of cements (ed. Bensted and Barnes), Spoon Press,
London, 2002.
13
Paper V - Investigation of early age deformation in SCC
[4] Barcelo, L., Moranville, M., and Clavaud, B., 'Autogenous shrinkage of concrete: a balance
between autogenous swelling and self-desiccation', Cement and Concrete Research, Vol. 35
(2005), pp. 177–183.
[5] Jensen O. M., Hansen F., 'A dilatometer for measuring autogenous deformation in hardening
Portland cement paste', Materials and Structures, Vol. 28 (181), pp. 406-409, 1995.
[6] Johansen, R. and Dahl, P.A., 'Control of plastic shrinkage of cement'. Paper presented at the 18th
Conference on Our World in Concrete and Structures, Singapore, 1993.
[7] NORDTEST NT BUILD 433, 'Concrete: Cracking Tendency – Exposure to Drying During the
First 24 Hours'. NORDTEST (Espoo, Finland, 1995).
[8] Holt, E.E., 'Early age autogenous shrinkage of concrete'. Technical Research Centre of Finland,
VTT Publication 446 (2001), Espoo, 184 pp.
[9] Bjøntegaard Ø., Hammer T.A., and Sellevold E.J., 'Cracking in High Performance Concrete
before Setting', Proceedings of the Int. Symposium on High-Performance and Reactive Powder
Concretes, Sherbrooke, Aug. 1998.
14
Paper VI - Effect of limestone filler BET(H2O)-area on
the fresh and hardened properties of SCC
Esping O., “Effect of limestone filler BET(H2O)-area on the fresh and hardened
properties of self-compacting concrete”, Submitted for publication in Cement and
Concrete Research, 2007.
Paper VI - Effect of limestone filler BET(H2O)-area on
the fresh and hardened properties of SCC
Paper VI - Effect of limestone filler BET(H2O)-area on
the fresh and hardened properties of SCC
Abstract
This paper presents a study on the use of limestone fillers with different specific surface area and their effect on
the fresh and hardened properties of self-compacting concrete (SCC). The surface area was determined by a
simplified BET method using water vapour as adsorbate. A rheometer and a slump flow test were used to measure
the flowability of fresh concrete. A concrete dilatometer was used to measure the autogenous shrinkage, and a ring-
test for the plastic cracking tendency. The compressive strength was determined at 28 days. It was found that the
measure of BET(H2O)-area can be used to evaluate the water requirement for constant workability of the SCC,
where a change in BET(H2O)-area of 1 000 m2/kg corresponds to approximately 0.8% in moisture content. The
results showed that filler with a large area will result in an increased autogenous shrinkage, decreased evaporation,
lower plastic cracking tendency, and a higher compressive strength. With additional water the results was the
opposite.
1
Paper VI - Effect of limestone filler BET(H2O)-area on
the fresh and hardened properties of SCC
underpressure in the skeletal structure will cause an surface area by Blaine fineness. Due to the
external deformation [9]. The pattern of autogenous methodology where the specific surface area is
deformation, exampled in Fig. 1, comprises three determined from air permeability, based on packed
distinct stages which can be defined as plastic, spherical particles, information about the shape,
semiplastic and rigid, separated by the time to initial texture and surface porosity is neglected [28,32].
and final set [11,12]. Other possibly more correct methods, such as the
BET with nitrogen gas and image analysis, are more
Plastic Semiplastic Rigid Self-supporting seldom used due to their complexity and costs.
skeleton starts to form
In this work, the effect of the specific surface area
Deformation, Pressure & Temp
Initial set
of different limestone fillers on the fresh and
Final set hardened properties of self-compacting concrete
Pore pressure (SCC) has been experimentally evaluated. The
(measured)
investigated properties were rheology, autogenous
Autogenous defor-
mation (measured) deformation, plastic cracking tendency and
Temperature compressive strength. The surface area was
(measured) determined by a simplified BET method, using water
Chemical shrinkage vapour as adsorbate. The change in BET(H2O)-area
0 ~6 ~12 ~18 ~24 (assumed) was translated to a change in water demand for the
Time (from mix) [hours]
concrete mix to maintain a constant workability,
Fig. 1. Typical early-age linear autogenous deformation
and corresponding development of temperature and based on the assumption that 30 full molecular layers
capillary pore pressure (based on measures of a SCC w/c of water covering the particle surface are required to
0.45, from [12]). decrease interactions and provide sufficient
lubrication for flowability.
The physical nature of better packing, by addition
of filler material, will not only govern the concrete
flowability, but also the compressive strength due to 2. Materials and mix design
the denser matrix and the better dispersion of cement
grains [13-16]. Furthermore, the surfaces of the filler The mix design and its constituents, as used in this
material will act as nucleation sites for the early study, comprise typical materials and compositions
reaction products of CH and CSH, which will for self-compacting concrete with w/c 0.55 in
accelerate the hydration of cement clinkers Sweden. The cement was a type CEM II/A-LL
(especially C3S) and consequently increase the early 42.5R, the fine aggregate a 0-8 mm natural ground
age compressive strength [17-20]. The effect of gravel, the coarse aggregate a 8-16 mm crushed
nucleation on the strength is dependent on the filler’s granite stone and the superplasticizer a
affinity to cement hydrates, and it increases with polycarboxylate ether-based type. Five ground
fineness and specific surface area of the filler. limestone fillers, with similar chemical composition
Limestone filler is not pozzolan, but nor fully inert as but different size distributions and specific surface
it reacts with the alumina phases of the cement. If the areas, were used. The area was determined by
cement has a significant amount of tricalcium BET(H2O); A simplified method, based on the BET
aluminate (C3A), calcium carboaluminate will be theory [33], where the area was determined
produced from the reaction between calcium gravimetrically on conditioned samples at different
carbonate (CaCO3) from the limestone and the C3A relative humidities and deduced from the adsorbed
[21-27]. This reaction, accelerating the hydration and volume of water molecules required to cover and
increasing the compressive strength, increases with form a monolayer on the surface of the sample
the C3A content of the cement and the fineness and [28,34-37]. The measured BET(H2O)-area (SBETH2O),
specific surface area of the filler. the area by Blaine (SBlaine) and the calculated area
from size distribution (SSize) [34,37] for the five
Since the ratio of surface area to volume increases limestone fillers are given in Fig. 2. The size
exponentially with particle irregularity (shape, distribution, measured with a Malvern laser
texture and porosity) and decreased size, and as this diffraction instrument, is presented in Fig. 3. The
area has a predominating effect on fresh and limestone filler named L40 has the smallest BET-
hardened concrete [28-31], quantification of area, and is used as a reference. It can be noted that
geometrical properties of fillers and fines is essential. the filler named L70 is the coarsest, but has the
Powder material (filler, cement, etc.) is traditionally largest BET-area.
characterized by the size distribution and the specific
2
Paper VI - Effect of limestone filler BET(H2O)-area on
the fresh and hardened properties of SCC
The BET(H2O)-area for the gravel is ~2800 m2/kg, flowability. In Table 1 the changes in mixing water
and the BET(N2)-area for the cement is ~2000 m2/kg. due to differences in specific area of limestone filler,
For cement the BET(H2O) method is not valid. Due using L40 as reference, are given.
to the differences in size and polarity of the water
and nitrogen molecule the area by BET(H2O) is Table 1. Mixing water, in litre/m3, with compensations for
larger than by BET(N2) [37]. With a linear the differences in specific surface area of limestone fillers.
relationship of 1.55 [12], the BET(H2O)-area for the The L40 with the smallest BET area is used as reference.
cement can be estimated to 3100 m2/kg. L40 (ref) L15 L70 G100 G200
187.00 187.68 192.89 187.12 187.02
8 000 800 (+0.68) (+5.89) (+0.12) (+0.02)
6 000 600
2
The concrete was prepared in batches of 40 litres,
2
3
Paper VI - Effect of limestone filler BET(H2O)-area on
the fresh and hardened properties of SCC
3.2. Autogenous deformation test method addition, and the sample was exposed to an air
velocity of 4.5 m/s with 23±2ºC and 35±5% RH.
The autogenous linear deformation was monitored Temperature, pore pressure and weight loss
by a concrete digital dilatometer (CDD), able to (evaporation) in the concrete specimens, and the
measure before setting when concrete is fresh [12]. strain in the inner ring, were continuously recorded.
The method is a modification of the CT1 dilatometer After 20 hours of drying the crack index was
for pastes and mortars by Jensen & Hansen [38]. The measured as the average (of three specimens) total
CDD setup consists of a concrete specimen cast in a crack area (crack length × crack width) on the
steel coil-reinforced vapour-proof flexible PE-tube concrete surface.
with tight end-caps, a measuring rig in stainless steel,
and a digital gauge (3 µm accuracy) recording the Steel rings (Ø300/600) Sample Stress raisers
unrestrained linear deformation; see Fig. 5. The test, Fan Base plate (steel) Cracks
Fig. 5. The Concrete Digital Dilatometer (CDD) for linear 3.4. Compressive strength test
autogenous deformation measurement (from [12]).
Compressive strength was measured on 150 mm
Due to greater stiffness in the radial than in the cubes after 28 days, in accordance with EN 12390-
longitudinal direction of the mould, in fluid state, the 1,-2 and -3. All presented values of compressive
flexible mould transforms a large part of the strength (fc) are normalized to a porosity of 4%. Due
volumetric deformation into a linear deformation. As to the differences in limestone fillers’ BET-area the
the concrete undergoes transition from a fluid to a flowability was not consistent between the mixtures;
rigid state, the deformation becomes isotropic. Based hence also the air content was not equal. A series of
on empirical evaluation, the ratio between linear and corresponding mixes with different air content, in the
volumetric deformation for a liquid is approximately range of 0-5%, were made in order to evaluate the
0.8 [39]. No correction for this was made as the effect of air content (porosity) on the compressive
setting point is not a well-defined physical state but strength. This was made in accordance with the
rather a continuous transformation from liquid to a general equation for ceramic materials [41]:
solid state. f c = f c 0 ⋅ e k ⋅ P (Eq. 2). The porosity, P, was
The experiments were supplemented with determined by the measured density in fresh and
measurements of temperature and pore pressure hardened states (according to EN 12350-6 and EN
placed in the centre of the core. The pressure 12390-7), together with the measured air content by
transducers were connected to a de-aired water-filled pressure test (EN 12350-7). The compressive
system with a needle (internal diameter of 0.4 mm strength “without” pores, fc0, was 55.0 MPa for the
and 50 mm length). concrete de-aired in a vacuum desiccator for 30
minutes before moulding. The constant k was
3.3. Ring- test method for plastic shrinkage cracking empirically evaluated to 6.5.
4
Paper VI - Effect of limestone filler BET(H2O)-area on
the fresh and hardened properties of SCC
7 min
despite the fact that “L70” is coarser, it generates a
400
larger specific area and thereby a stiffer consistency,
60 min and has a larger water demand. This might be
200
explained by the filler’s geological origin and age,
where “L70” has a rougher and more porous particle
0 surface.
600
4.2. Autogenous deformation
450
Yield stress [Pa]
5
Paper VI - Effect of limestone filler BET(H2O)-area on
the fresh and hardened properties of SCC
-6
Fig. 9. The limestone filler’s BET(H2O)-area and the L40
0
evaluated rate of autogenous deformation from autogenous G100
deformation in the plastic and semiplastic period. G200
-400
Furthermore, Fig. 10 shows the development of the
measured pore pressure, and Fig. 11 the evaluated -800
maximum rate of pore pressure which occurred at 7- 0 6 12 18 24
8 hours from mixing [43]. The point of maximum Time (from mix) [hour]
underpressure could not be evaluated due to the loss Fig. 12. Sealed (“autogenous”) deformation for the
of pressure at random times. This effect is usually mixtures where the cement was replaced with equal
referred to as the breakthrough pressure [5]. It can be volume filler (from [43]).
noted that the rate of pore pressure, and rate and
magnitude of autogenous deformation, showed to The hydration process (generating chemical
correlate with the limestone fillers’ BET(H2O)-area. shrinkage) is generally considered to be the driving
0 force of autogenous deformation; hence the term
G200 “autogenous” in this case might be incorrect. Even
Pore pressure [kPa]
-60
2
SBETH2O [m /kg]
Fig. 11. The limestone filler’s BET(H2O)-area and the
evaluated maximum rate of pore pressure (at 7-8 hours
from mixing).
6
Paper VI - Effect of limestone filler BET(H2O)-area on
the fresh and hardened properties of SCC
4.3. Plastic shrinkage cracking The differences in crack tendency are most likely a
consequence mainly of evaporation, which is verified
A representative measure (from [43]) showing the by the initial rate of measured evaporation (up to 4
relationship between the development of strain, hours from mix, before initial setting) in Fig. 15. A
temperature, and pore pressure (at 20 and 60 mm large particle surface area lowers the evaporation,
depth) for one of the concretes exposed to drying is whereas extra water increases the
shown in Fig. 13. As can be seen, the pore pressure evaporation.
develops more rapidly in comparison with the sealed 0.44
samples, in Fig. 10. The maximum underpressure is
2
Additional water
30 minutes between the two depths. The measured 0.42
strains indicate that cracking was initiated at 3-4
No compensation
hours from mixing [43]. The average crack area is
presented in Fig. 14, where it can be seen that the 0.40
crack tendency is lower for concrete incorporating
filler with a high BET(H2O)-area, and that, when
adding extra water to compensate for the loss in 0.38
flowability, the crack tendency increased 0 2000 4000 6000 8000
2
significantly. An increase in filler’s BET(H2O)-area SBETH2O [m /kg]
of 1000 m2/kg results in ~20% less cracking Fig. 15. Initial rate (<4 hours from mix) of evaporation,
tendency. without and with extra water added to compensate for the
Max BET(H2O)-area.
Additional water
60
accelerated hydration due to nucleation). But as the
filler with the largest area (“L70”) also was the
coarsest, the increased strength can also be attributed
40
No compensation to the filler’s porosity increasing its absorption of
water and consequently reducing the effective
20 water/cement ratio. A change in BET(H2O)-area by
1000 m2/kg proved to correspond to ~0.15 MPa in
0 compressive strength for a SCC with 160 kg
0 2 000 4 000 6 000 8 000 limestone fillers (i.e. ~1 kPa/kg filler).
2
SBETH2O [m /kg] That the porosity (accessible to water absorption) is
incorporated in the BET-area is confirmed by the
Fig. 14. The limestone filler’s BET(H2O)-area and the
plastic shrinkage crack area, without and with extra water measured “autogenous” deformation on the mixtures
compensating for the differences in BET-area (“L40” as without cement (Fig. 12), where the mixture with
reference). “L70” generated the largest shrinkage (and swelling).
7
Paper VI - Effect of limestone filler BET(H2O)-area on
the fresh and hardened properties of SCC
compensation.
No compensation o The mixtures where the cement was replaced
47 with limestone filler generated an “autogenous”
shrinkage of ~0.8 mm/m at 24 hours, counted
after an initial swelling up to 4 hours. The
46 magnitude of deformation (both swelling and
shrinkage) corresponded to the limestone filler’s
Additional water
BET(H2O)-area.
45
0 2000 4000 6000 8000
2
SBETH2O [m /kg] References
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9
Paper VI - Effect of limestone filler BET(H2O)-area on
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10