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Quantification of the shape of particles for calculating specific surface area of

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Conference Paper · January 2016

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 International RILEM Conference on Materials, Systems and Structures in Civil Engineering
Conference segment on Simulation tools used in the execution phase of Concrete Structures
22-24 August 2016, Technical University of Denmark, Lyngby, Denmark

QUANTIFICATION OF THE SHAPE OF PARTICLES FOR

CALCULATING SPECIFIC SURFACE AREA OF POWDERS
Yahya Ghasemi (1), Mats Emborg (1)(2), Andrzej Cwirzen (1)

(1) Luleå technical university, Luleå, Sweden

(2) Betongindustri AB, Stockholm, Sweden

Abstract
The concepts of particle packing and water/paste layer theories are commonly used for basis
of concrete mix design models. While particle packing insists on achieving fewer voids in
aggregate matrix by e.g. adding fine aggregates, water/paste layer theories state that
increasing the amount of fines will lead to higher water demand since the specific surface area
of particles will increase. In order to calculate the thickness of excess paste in water/paste
layer theories, it is essential to have an estimation of specific surface area of the particles.
However, the complexity of the instruments required to measure specific surface area makes
the methods costly and also causes an issue regarding the availability of the instruments
leading to less popularity of water/paste layer theories compared to mix design approaches
based on the particle packing theory. Introducing a model that can roughly estimate the
specific surface area of particles may eliminate the need for measuring specific surface area
which in turn contributes to cost reduction and also laying a foundation for calculation of
water layer thickness.
The paper aimed to study calculated specific surface area by replacing regular convex
polyhedrons with actual particle shapes based on the size distribution curves of the samples
and to compare the results with data obtained by Blaine test.
The conducted study suggests that in most cases, assumption of spherical shape for the
particles leads to an acceptable estimation of SSA. However, SSA of powders with more
angular particles can be calculated more accurately with the assumption of Polyhedron shape
rather than spheres
 International RILEM Conference on Materials, Systems and Structures in Civil Engineering
Conference segment on Simulation tools used in the execution phase of Concrete Structures
22-24 August 2016, Technical University of Denmark, Lyngby, Denmark

1. Introduction

1.1. Background
During past decades, several attempts were made on formulating the mix design of concrete.
Most of these models are based on the assumption that the properties of concrete in fresh state
namely; flow properties and workability are chiefly governed by the particle size distribution
(PSD) and the particle packing [1-3]. According to the above-mentioned models, particle
packing can be increased by modifying PSD which in turn usually leads to increasing the
share of fines. Packing theory assumes that adding fine particles to a particle structure helps
fill up the voids in the particle structure leaving only minimum space for water. In this way
adding fine particles will reduce the water requirement [1,4,5]. However, the packing of
aggregate is dependent also on the shape of the aggregate particles. The effect of particle
shape is more difficult to comprehend and it is indirectly accounted for by measuring the
packing of mono- sized fractions.
Another approach to compiling a mix design model is based on excess paste/water layer
theories first introduced by [6]. A major hypothesis by [7] states that the relative slump of a
water-powder mixture becomes a function of the specific surface area (SSA) when sufficient
water is present to flow. Based on the hypothesis, a thin layer of adsorbed water molecules
around the particles is necessary to assure the flow characteristics of the hydrating system. It
is reported that the thickness of this water layer is related to sensitivity of the mix on changes
in the water content and also the specific surface area of the material used [7], as later
confirmed by [8]. Moreover, the water layer theory assumes that the water demand of a
mixture depends on the surface area of the particles in that mixture. Increasing the surface
area by adding small particles will increase the water requirement [9-13].
Both approaches (Particle packing and Water/paste layer theories) strongly depend on the
shape of the aggregate in one way or another, that is especially more essential when it comes
to water/paste layer theories which requires the specific surface area as an input for the model.
While it is possible to directly measure SSA, the complexity of instrument required for the
measurement imposes issues namely; the availability of the testing instruments and the cost. It
is also possible to estimate the SSA based on the assumption that particles have ideal
spherical shapes using the PSD data [14].
The paper aims at defining an alternative way to improve the accuracy of calculated SSA by
assuming ideal polyhedron shapes for the particles in addition to the previously mentioned
spherical shapes and by comparing the calculated SSA to the measurements obtained by
Blaine test. Accurate estimation of SSA can provide a tool for calculating water demand of
the powders at the on-set of flow and also can be used in water/paste layer theories.

1.2. Specific surface area (SSA)

The specific surface area is the quotient of the absolute available surface excluding all open
inner surfaces (pore walls) divided by the mass [m2/g]. For concrete mix design, only the
outer surface being in contact with water is of interest. With the consideration of the specific
density, the specific surface area could also be expressed as area per volume [m2/m3]. Besides
mass and solid volume, the SSA can also be related to a bulk volume (taking account for the
void fraction) or a cross-sectional area [8].
There are several ways of determining SSA based on direct and indirect measurements, e.g.
Blaine test, Lea and Nurse method. Both tests give closely similar results but are not
 International RILEM Conference on Materials, Systems and Structures in Civil Engineering
Conference segment on Simulation tools used in the execution phase of Concrete Structures
22-24 August 2016, Technical University of Denmark, Lyngby, Denmark

applicable to fine and ultra-fine powders. Another method that has been used to determine
SSA is the volumetric static multi-point method better known as the BET method [15].
However, determining the SSA value using the mentioned tests is associated with a highly
device- related complexity. An indirect possibility for determining the SSA can be its
deviation from the particle size distribution [14]. Assuming that all the particles are spheres,
total SSA for spherical particles can be calculated by Eq. (1).
𝑛𝑛
𝜔𝜔𝑖𝑖
𝑎𝑎𝑠𝑠𝑠𝑠ℎ = 6 � (1)
𝑑𝑑̅𝑖𝑖,𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎ℎ . 𝜌𝜌𝑠𝑠
𝑖𝑖=1
where:
𝜔𝜔𝑖𝑖 is the mass of a grain fraction i, being the mass percentage of the fraction between di and
di+1.
𝑑𝑑̅𝑖𝑖,𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎ℎ is the arithmetic mean diameter of fraction i and i+1.
𝜌𝜌𝑠𝑠 is the specific density of the particles.

1.3. Water/Paste layer theories

The paste layer theory originates in the design of self-compacting concrete. It is known that
cement paste should not only fill the voids among the aggregates but surround all particles
with a thin layer of paste to fulfill workability requirements [16]. The required amount of
paste for this layer depends on the specific surface area of the particles. The larger the surface
area of the particles, the smaller the thickness of the surrounding paste layer and the larger the
available surface for cement matrix–aggregate bond. The theory has proven useful in self-
compacting concrete [9,17].
In paste layer theory approach, the packing density of the aggregate is measured in order to
determine the amount of cement paste required to fill up the voids, the ramining paste added
in the mixture is considered as excess paste, Water layer theory follows a similar prinicple as
paste layer theory. Based on the excess water layer theory, the thickness of water layer can be
calculated by dividing the amount of water by available specific surface area of all the
particles including cement and other micro fines. see Figure 1.

Figure 1. Volume of water, divided into excess water and void filling water, within a concrete mixture
in a unit volume [12].
 International RILEM Conference on Materials, Systems and Structures in Civil Engineering
Conference segment on Simulation tools used in the execution phase of Concrete Structures
22-24 August 2016, Technical University of Denmark, Lyngby, Denmark

Estimation of specific surface area of particles plays a major role in calculation of thickness of
both paste and the water that surronds the particles.

2. Materials

In order to examine the accuracy of SSA calculation, the data needs to be compared to actuall
measurments of SSA; for this purpose, four powders were chosen and their properties namely
specific density, bulk density, Blaine value and their particle size distribution curves were
extracted from [10] and [18] and are represented in Table. 1.

Table 1: Densities and SSA of the powders.[10][18]

Specific density Loose packing Bulk density SSA based on
Material
(g/cm3) density (g/cm3) Blaine (cm2/g)
CEM III/B 42.5 N 2.96 0.72 2.13 4500
Marble Powder 2.80 0.64 1.79 4580
Limestone 2.21 0.69 1.87 4040
Quartz Powder 2.60 0.64 1.66 2600

Particle size distribution of the materials is an important factor in calculation of the specific
surface area, there are several methods for determining the PSD. The size distribution curve
was obtained by deploying low angle laser light scattering technique (LALLS) conducted by
[10]. See the particle size distribution curves of the selected powders in Figure 2.

100
90 CEM III 42,5N
80 Marble Powder
Cumulative finer (Vol. %)

70 Limestone
Quartz
60
50
40
30
20
10
0
0,1 1 10 100 1000
Particle size (micron)

Figure 2. Particle size distribution of the powders.[10][18]

 International RILEM Conference on Materials, Systems and Structures in Civil Engineering
Conference segment on Simulation tools used in the execution phase of Concrete Structures
22-24 August 2016, Technical University of Denmark, Lyngby, Denmark

Additionally, in order to further validate the relation between polyhedrons and the particle
shape and to be able to distinguish the difference in particle geometry, SEM micrographs
have been prepared by [10] and shown in Figure 3.

(a) CEM III/B 42.5 N (b) Dolomitic marble powder

(c) Limestone powder

Figure 3. SEM micrographs of the investigated powders, 1000X magnified.[10]

3. Computation of SSA based on particle size distribution

As mentioned before, using Eq. (1) it is possible to calculate SSA based on the particle size
distribution for spheres. In addition to sphere-based calculation of SSA, other polyhedrons
were examined to re-calculate the SSA. Table 2. shows the selected polyhedrons and their
geometrical properties.
 International RILEM Conference on Materials, Systems and Structures in Civil Engineering
Conference segment on Simulation tools used in the execution phase of Concrete Structures
22-24 August 2016, Technical University of Denmark, Lyngby, Denmark

Table 2: Polyhedrons used in the calculation of SSA.

Shape Surface Area Volume SSA/V

√2𝑎𝑎3 14.697
Tetrahedron √3𝑎𝑎2
12 𝑎𝑎

6
Cube 6𝑎𝑎2 𝑎𝑎3
𝑎𝑎
1
2√3𝑎𝑎2 √2𝑎𝑎3 7.348
Octahedron 3
𝑎𝑎

3 1 2.694
Dodecahedron �25 + 10√5𝑎𝑎2 (15 + 7√5)𝑎𝑎3
4 𝑎𝑎
5√3𝑎𝑎2 5 3.970
Icosahedron (3 + √5)𝑎𝑎3
12 𝑎𝑎
4𝜋𝜋𝑎𝑎3 3
Sphere 4𝜋𝜋𝑎𝑎2
3 𝑎𝑎

Replacing spheres with other polyhedrons will not only change the calculated volume and
specific surface area but also affects the pace of growth in SSA/Volume ratio according to
square-cube law.

3.1. Square-Cube law

The square-cube law was first introduced by Galileo [19] and it defines a mathematical
principle which describes the relationship between the volume and the area in accordance to
changes in size. According to the principle, as a shape grows in size, its volume grows faster
than its surface area. Consequently, as the size decreases its surface area grows faster than its
volume. The effect of square-cube law becomes especially significant for calculation of
specific surface area of finer particles namely powders and cement. Figure 4 illustrates the
difference in growth of SSA/Vol ratio of polyhedrons according to square-cube law.
 International RILEM Conference on Materials, Systems and Structures in Civil Engineering
Conference segment on Simulation tools used in the execution phase of Concrete Structures
22-24 August 2016, Technical University of Denmark, Lyngby, Denmark

400

350

300

250
Surface Area

200

150

100

50

0
0 50 100 150 200 250 300 350 400 450 500
Volume

Figure 4. Surface area against volume of the platonic solids and a sphere.

By writing Eq. (1) in its general form, the square-cube law effect can be implemented in the
equation.
𝑛𝑛
𝑆𝑆𝑆𝑆𝑆𝑆𝑖𝑖 . 𝜔𝜔𝑖𝑖
𝑎𝑎𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝 = � (2)
𝑉𝑉𝑖𝑖 . 𝜌𝜌𝑠𝑠
𝑖𝑖=1

where:
SSAi/Vi is the specific surface area to volume ratio of fraction i and is related to the shape as
shown in table 2.
To define the equivalent polyhedron to the spheres, it was assumed that the polyhedrons have
the same volume as the retained spheres on each fraction. The length of the sides of
polyhedrons is calculated based on the mentioned assumption. The average diameter of the
spheres in each fraction is determined based on the arithmetic mean approach.
 International RILEM Conference on Materials, Systems and Structures in Civil Engineering
Conference segment on Simulation tools used in the execution phase of Concrete Structures
22-24 August 2016, Technical University of Denmark, Lyngby, Denmark

4. Results and discussion

Calculated specific surface area according to Eq (2) and their corresponding Blaine values
from laboratory tests [10][18] are presented in Table 3.

Table3: Surface area of the powders and the deviation from the calculated SSA
Specific surface area (cm2/g)
Material Blaine

CEMIII/B42.5 4500 6892 5737 5469 5078 4927 4625

Marble 4580 4766 3968 3784 3515 3406 3199
Limestone 4040 7689 6401 6103 5668 5495 5160
Quartz 2600 4031 3355 3200 2964 2881 2705

Calculated values of SSA in case of CEMIII/B42.5, Limestone powder, and Quartz powder
were overestimated by 2.7%, 27% and 4%, respectively, in comparison to their corresponding
Blaine values. The high margin of error for Limestone powder can be related to the principles
of the Blaine method as it is a relative test which depends on the shape of the particles and the
compaction level or porosity of their compacted bed [20][21].
It should be noted that the model overestimated SSA in most of the studied materials. For the
case of Marble powder, calculations based on Tetrahedron shape for particles give a closer
estimation of SSA compared to the other platonic solids.

5. Conclusion

5.1. Analysis of the model

While it is shown that using the water layer theory can be a helpful tool for prediction of
flowability of concrete [9], the complexity of instruments required for measuring the SSA as
an essential input in the water layer theory model makes this approach less favoured by the
industry comparing to the mix design models based on particle packing. Thus formulating an
equation that can predict SSA using simple input data, the water layer theory can be used with
more simplicity and efficiency as a tool for anticipating the workability of the concrete.
The conducted study suggests that in most cases, assumption of spherical shape for the
particles leads to an acceptable estimation of SSA. However, SSA of powders with more
angular particles can be calculated more accurately with the assumption of Polyhedron shape
rather than spheres as it was the case for the Marble powder. See Figure 3 and Table 3.

5.2. Future work

More data is required in order to categorize the shape of particles based on the suggested
polyhedrons. In addition, since the Blaine test will result in relative values for powders other
than cement, an accurate method of measuring SSA of particles is necessary to calibrate the
 International RILEM Conference on Materials, Systems and Structures in Civil Engineering
Conference segment on Simulation tools used in the execution phase of Concrete Structures
22-24 August 2016, Technical University of Denmark, Lyngby, Denmark

model, e.g. microtomography. As a next step in the study, the actual SSA can be measured
using 3D models of the particle structure generated by microtomography scanning and can be
compared with the results obtained from the model. Moreover, the effect of changes in PSD
can be studied by modifying the distribution curves of the particle to a target curve.

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 International RILEM Conference on Materials, Systems and Structures in Civil Engineering
Conference segment on Simulation tools used in the execution phase of Concrete Structures
22-24 August 2016, Technical University of Denmark, Lyngby, Denmark

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