buildings

Article
Utilization of Quarry Dust and Calcareous Fly Ash for
the Production of Lightweight Cellular
Micro-Concrete—Synthesis and Characterization
Athanasia Soultana * and Michael Galetakis
School of Mineral Resources Engineering, Technical University of Crete, 73100 Chania, Greece;
[email protected]
* Correspondence: [email protected]




Received: 27 October 2020; Accepted: 23 November 2020; Published: 25 November 2020


Abstract: This study aims to assess the production of cellular micro-concrete, consisting of quarry dust,
calcareous fly ash, cement, and aluminum powder as aerating agent. The proposed mixture design
methodology is based on a Box–Behnken fractional factorial experimental design. Testing of specimens
included compressive and flexural strength, density, water absorption, and thermal conductivity
measurements. Results indicate that density is a characteristic property which determines all the
measured properties. Aerating agent to cement and fly ash ratio has the strongest effect on all the
measured properties. The developed methodology is a valuable tool for the production of cellular
micro-concrete with predetermined properties by utilizing large amounts of quarry dust.

Keywords: quarry dust; calcareous fly ash; cellular micro-concrete; Box–Behnken factorial design

1. Introduction
Aggregate quarrying operations such as crushing, sieving, etc., are used to produce large quantities
of fine by-products (<63 µm) known as quarry dust [1]. These fine by-products are difficult to handle
and pose several environmental, health, and operational issues [2,3].
Disposal of quarry dust is one of the most critical problems facing the quarrying industry, since,
on a number of occasions, quarry dust landfills may involve more space than the total of quarrying
operations [4]. Using a large amount of quarry dust in construction applications could be a feasible
solution to this problem, leading to both economic and environmental benefits for the quarrying
sector. Even though there have been various proposed methods for the utilization of these by-products,
they still remain under-utilized [1].
Over the past few years, there have been made many research efforts concerning the utilization
of quarry dust as sand substitution material (partial or total replacement) for the production of
several types of concrete and building elements [1,3–14]. However, the usage of quarry dust in
these applications is rather demanding with regard to compositional aspects. More specifically,
partial replacement of sand by quarry dust (up to 20% replacement) for the production of concrete
and cement-based products improves the mechanical and durability properties, but the addition of
higher quantities of quarry dust raises the water demand of the mixture. The large surface area of
fines increases the water required in order to maintain proper workability of the mixture, resulting in
higher shrinkage and strength deterioration [15]. However, the usage of effective superplasticizers,
which reduce the required water amount, and sophisticated mixture design methodologies makes the
incorporation of quarry dust in concrete and cement-based building elements possible [8].
Galetakis and Soultana [8] showed that the majority of research studies related to the exploitation of
quarry dust as raw material in the construction sector refer to the production of self-compacting concrete

Buildings 2020, 10, 214; doi:10.3390/buildings10120214 www.mdpi.com/journal/buildings

Buildings 2020, 10, x FOR PEER REVIEW 2 of 18

Galetakis
Buildings 2020, 10, and
Soultana [8] showed that the majority of research studies related to 2 the
214 of 17
exploitation of quarry dust as raw material in the construction sector refer to the production of self-
compacting concrete and ordinary concrete products, while some of them study the production of
and ordinary concrete products, while some of them study the production of cement-based building
cement-based building elements like masonry bricks and artificial stones (Figure 1). On the other
elements like masonry bricks and artificial stones (Figure 1). On the other hand, research studies
hand, research studies related to the use of quarry dust for the production of lightweight structural
related to the use of quarry dust for the production of lightweight structural elements such as aerated
elements such as aerated concrete are very limited [4–8].
concrete are very limited [4–8].

Figure 1. Proposed uses of quarry by-products. Based on Galetakis and Soultana [8].
Figure 1. Proposed uses of quarry by-products. Based on Galetakis and Soultana [8].
Aerated concrete is a lightweight cellular material consisting of ultrafine aggregates (finely crushed
quartz sand) and is therefore called cellular micro-concrete (CMC). Besides finely ground quartz
Aerated concrete is a lightweight cellular material consisting of ultrafine aggregates (finely
sand, cement, lime, and a small amount of aluminum powder as aerating agent are also used for its
crushed quartz sand) and is therefore called cellular micro-concrete (CMC). Besides finely ground
production. It is homogeneous compared to conventional concrete, with a significantly lower density.
quartz sand, cement, lime, and a small amount of aluminum powder as aerating agent are also used
It also has high workability and excellent thermal insulating properties [16].
for its production. It is homogeneous compared to conventional concrete, with a significantly lower
Its cellular structure (Figure 2) is obtained through a gas-producing chemical reaction, as shown
density. It also has high workability and excellent thermal insulating properties [16].
in Equation (1). The mechanism of the hydrogen-generating reaction takes place in four stages and
Its cellular structure (Figure 2) is obtained through a gas-producing chemical reaction, as shown
includes the destruction of the passive layer at the surface of aluminum powder, the formation of katoite
in Equation (1). The mechanism of the hydrogen-generating reaction takes place in four stages and
crystals, aluminum hydration, and the release of hydrogen [17]. Following the reaction, CMC can
includes the destruction of the passive layer at the surface of aluminum powder, the formation of
be cured under hydrothermal conditions at 180–200 ◦ C using high-pressure steam (autoclaved) or
katoite crystals, aluminum hydration, and the release of hydrogen [17]. Following the reaction, CMC
moist-cured (non-autoclaved) [7,16].
can be cured under hydrothermal conditions at 180–200 °C using high-pressure steam (autoclaved)
or moist-cured (non-autoclaved) [7,16].
2Al + 3Ca(OH)2 +6H2 O → 3CaO·Al2 O3 ·6H2 O + 3H2 (gas) (1)
2Al + 3Ca(OH)2 +6H2O → 3CaO·Al2O3·6H2O + 3H2(gas) (1)
Although the autoclaving process gives rise to crystallization and thus high compressive strength
early on, this process is energy-intensive (typically reaching a temperature of 180–200 ◦ C and a pressure
of 4–16 bar) and requires a large amount of quartz sand that must be finely ground. Crushing quartz
sand, as well as curing CMC, using autoclaving processes, is energy-intensive, so it is important to
study the possibility of producing CMC by using other materials instead of quartz sand and less
energy-intensive production procedures. Moreover, the fine-grained airborne quartz dust (also known
as respirable crystalline silica in occupational hygiene) is a harmful substance if inhaled by humans [18].
Thus, its substitution by an inert substance, such as a quarry dust consisting mainly of calcite,
is highly desirable.
Fly ash produced by lignite combustion for the production of electricity is also an important
by-product. It is derived from coal-fired power stations, it has pozzolanic and/or hydraulic properties,
and its composition is defined as a calcium-alumino-silicate. The use of fly ash can improve many
properties of fresh and hardened concrete and contribute to lower energy consumption and reduced CO2
Buildings 2020, 10, 214 3 of 17

emissions [19,20]. In particular, the addition of siliceous fly ash improves workability, increases plasticity,
and reduces water demand of the mixture, due to its fineness and the spherical shape of its grains [21].
However, a siliceous fly ash replacement of cement greater than 20% to 30% results in a reduction in
the mechanical strength of the produced mixtures, especially at early stages due to the reduction in the
pozzolanic activity of the mixture [19,21]. On the other hand, the addition of calcareous fly ash leads
to reduced workability and higher water demand, but it also enhances mechanical strength at early
stages [22,23]. Calcareous fly ashes are rich in free lime and so it is estimated that they can be used for
the total2020,
Buildings substitution of lime,
10, x FOR PEER which is used in CMC production using Al powder as an aerating 3agent.
REVIEW of 18

Figure 2.
Figure 2. Porous
Porous structure
structure of
of CMC.
CMC.

Although
This studythe aimsautoclaving
to assess the process gives rise
simultaneous usetoofcrystallization
calcareous fly and thusquarry
ash and high compressive
dust for the
strength early
production on, this
of CMC. More process is energy-intensive
specifically, it aims to assess(typically reachingofaCMC
the production temperature
optimized of for
180–200 °C
strength
and adensity,
pressure of 4–16 bar)
consisting and requires
of cement, calcareousa largeflyamount
ash, and of high
quartz sand that
amounts of must
quarry bedust
finely ground.
under the
Crushing quartz
conventional sand,
curing as wellused
process as curing CMC, using autoclaving
for cement-based building elementsprocesses, ± 2 ◦ C and a relative
is energy-intensive,
(at 20 so it
is important
humidity toleast
of at study 95%theforpossibility
28 days).ofThe producing CMCofbyoptimal
achievement using other
valuesmaterials
of strengthinstead of quartz
and density is
sand and lessthus,
challenging; energy-intensive
a specialized production
mixture design procedures. Moreover,
methodology basedtheonfine-grained
the Box–Behnken airborne quartz
fractional
dust (also
factorial known
design as respirableiscrystalline
of experiments proposed.silica in occupational hygiene) is a harmful substance if
inhaled by humans
Factorial design[18]. Thus, its substitution
of experiments is widely used by anfor
inert substance,
product such asin
optimization a quarry
several dust consisting
manufacturing
mainly of calcite,
processes [24–28].is The
highly mostdesirable.
common factorial designs used in optimization are the three-level
Fly ash produced
full factorial design, the by lignite
centralcombustion
compositefor the production
designs (CCD), and of electricity is also an important
the Box-Behnken by-
(BB) designs.
product.
Full It is derived
three-level factorialfrom coal-fired
design requirespower stations,
a large numberit has
of pozzolanic
experimentsand/orwhenhydraulic
dealing with properties,
a great
and its composition
number of factors. In is such
defined as a calcium-alumino-silicate.
cases, subset of full factorial design, The use of flytoash
referred as can improve
fractional many
factorial
properties
design, of fresh
is used. Theand hardened concrete
Box–Behnken design used and contribute
in this study to is
lower energy consumption
a three-level and reduced
fractional factorial design
CO2 constitutes
and emissions [19,20].
a quickInand particular, the addition
cost-effective methodoftosiliceous
study the flyjoint
ash improves workability,
effect of design factorsincreases
with the
plasticity, and
minimum reduces
number water demand
of experiments [29].ofReaders
the mixture, due to
interested inits fineness
factorial and the
design spherical shape
of experiments couldof
its grains
refer [21]. However, a siliceous fly ash replacement of cement greater than 20% to 30% results in
to [30].
a reduction in the mechanical strength of the produced mixtures, especially at early stages due to the
2. Materials
reduction in and
the Methods
pozzolanic activity of the mixture [19,21]. On the other hand, the addition of
calcareous fly ash leads to reduced workability and higher water demand, but it also enhances
2.1. By-Product Characterization
mechanical strength at early stages [22,23]. Calcareous fly ashes are rich in free lime and so it is
Quarry
estimated thatdust
theyused
can inbe this
usedstudy
for the comes
total from a dry mortar
substitution of lime,plant
whichlocated
is usedinintheCMCisland of Crete
production
(Chania,
using Al Greece).
powder as More specifically,
an aerating it was collected through the de-dusting process of mortar-grade
agent.
crushed
Thismarble
study sand
aimsby to post
assessdryer
the air cyclones. Calcareous
simultaneous fly ash originates
use of calcareous fly ash andfromquarry
a coal dust
power plant
for the
located at Agios Dimitrios in Kozani area (Kozani, Greece).
production of CMC. More specifically, it aims to assess the production of CMC optimized for strength
and density, consisting of cement, calcareous fly ash, and high amounts of quarry dust under the
conventional curing process used for cement-based building elements (at 20 ± 2 °C and a relative
humidity of at least 95% for 28 days). The achievement of optimal values of strength and density is
challenging; thus, a specialized mixture design methodology based on the Box–Behnken fractional
factorial design of experiments is proposed.
Factorial design of experiments is widely used for product optimization in several
crushed marble sand by post dryer air cyclones. Calcareous fly ash originates from a coal power plant
located at Agios Dimitrios in Kozani area (Kozani, Greece).
Both fly ash and quarry dust were characterized for their particle size distribution and their
mineralogical composition. Particle size was determined by a laser particle size analyzer (Malvern
Instruments, Mastersize-S, Malvern, UK). Mineralogical analysis was performed using an X-ray
Buildings 2020, 10, 214 4 of 17
diffractometer (Bruker AXS, D8-Advance, Billerica, MA, USA) with a Cu tube and a scanning range
from 4° to 70° 2-theta (θ), with a step 0.02° and 0.2 s/step measuring time.
The
Bothgrain sizeand
fly ash distribution of the
quarry dust quarry
were dust and the
characterized forfly ash particle
their used is shown in Figure 3.and
size distribution As seen
their
in Figure 3, thecomposition.
mineralogical median particle size for
Particle quarry
size dust and flyby
was determined asha is 48 and
laser 20 μm,
particle sizerespectively.
analyzer (Malvern
RegardingMastersize-S,
Instruments, quarry dust, Malvern,
mineralogicalUK).analysis (Figureanalysis
Mineralogical 4) showed wasthat it consistsusing
performed of 97%ancalcite
X-ray
(CaCO 3), 2% dolomite
diffractometer (Bruker(CaMg(CO 3)2), and 1%
AXS, D8-Advance, quartz MA,
Billerica, (SiO2USA)
). with a Cu tube and a scanning range
fromFigure
4◦ to 705 ◦and Table
2-theta 1 present
(θ), the 0.02
with a step XRD◦ and
pattern and the
0.2 s/step mineralogical
measuring time. composition of the fly ash
used,Therespectively.
grain size distribution of the quarry dust and the fly ash used ishigh
As seen in Table 1 and Figure 5, fly ash contains a amount
shown of CaO
in Figure (22%)
3. As seenas in
free lime
Figure 3, and so it canparticle
the median be usedsize
for for
the quarry
total substitution
dust and fly ofash
limeis for the production
48 and of CMC.
20 µm, respectively.

100
Quarry dust
90 Fly ash
80
Cumulative passing (%)

70
60
50
40
30
20
10
0
0.01 0.1 1 10 100 1000
Particle size (μm)

Figure 3. Particle size distribution of quarry dust and fly ash used.
Figure 3. Particle size distribution of quarry dust and fly ash used.
Regarding quarry dust, mineralogical analysis (Figure 4) showed that it consists of 97% calcite
Buildings 2020, 10, x FOR PEER REVIEW 5 of 18
(CaCO3 ), 2% dolomite (CaMg(CO3 )2 ), and 1% quartz (SiO2 ).

Figure 4. XRD pattern of quarry dust.

Figure 4. XRD pattern of quarry dust.

Figure 5 and Table 1 present the XRD pattern and the mineralogical composition of the fly ash
used, respectively. As seen in Table 1 and Figure 5, fly ash contains a high amount of CaO (22%) as free
lime and so it can be used for the total substitution of lime for the production of CMC.
Buildings 2020, 10, 214 5 of 17
Figure 4. XRD pattern of quarry dust.

Figure 5.
Figure XRD pattern
5. XRD pattern of
of fly
fly ash.
ash.

Table 1. Mineralogical composition of fly ash.

Table 1. Mineralogical composition of fly ash.
Mineral wt%
Mineral wt%
L: Lime, CaOCaO
L: Lime, 22 22
A: Anhydrite, CaSO4 7
A: Anhydrite, CaSO4
C: Calcite, CaCO3
7 24
C: Calcite,
B: Brownmillerite, Ca2CaCO
(Al,Fe)32 O5 24 7
B: Brownmillerite,
Q: Quartz, SiOCa2 2(Al,Fe)2O5 7 7
G: Gehlenite, Ca2 Al2SiO
Q: Quartz, SiO27 7 4
At: Anorthite, CaAl2 Si2 O8
G: Gehlenite, Ca2Al2SiO7 4 6
H: Hematite, Fe2 O3 1
At:
La: Anorthite, CaAl2Si2O8
Larnite, Ca2 SiO 6 2
4
H: Hematite,
Amorphous material Fe2O3 1 20
La: Larnite, Ca2SiO4 2
2.2. Cement Type and Admixtures Amorphous material 20

In thisType
2.2. Cement study,
andordinary Portland cement type CEM I 42.5N complying with EN 197-1 was
Admixtures
used in various proportions. In order to reduce the water demand and improve the rheological
characteristics of the mixture, a polycarboxylate-based superplasticizer type Melflux 2651F was also
used. A limestone–aluminum mixture type RO 260 composed of 10% aluminum powder and 90%
limestone powder was used as an aerating agent in various proportions. The aerating agent used had
an average diameter of around 45 µm and a high specific surface area (~19,000 cm2 /g).

2.3. Mixture Design Methodology

At first, the ingredient proportions and admixture dosages were chosen based on a series of
preliminary tests, where material availability, economic, technical, and environmental factors, as well
as existing studies were taken into consideration [1,8,23,31]. More specifically, cement proportions
were chosen to vary between 12 and 22 wt%, fly ash proportions ranged from 8 to 15 wt%, quarry dust
ranged between 31 and 53 wt%, while aerating agent and superplasticizer dosages were chosen based
on the manufacturer’s recommendations and varied between 1.3 and 3 wt% and between 0.08 and
0.16 wt%, respectively.
As already mentioned in Section 2.1, the fly ash used contains a high amount of CaO (22%),
which leads to the fast setting of the mixtures and higher water demand [22,23]. For a given mixing
and molding time, fast setting of the mixtures requires higher amounts of water in order to maintain
the slurry properties. For this reason, a SOWER high speed mixer (0–8000 rpm) was used for the
Buildings 2020, 10, 214 6 of 17

production of the mixtures in order to achieve short mixing time (20–40 s), reduce the required water
content, and achieve high grain dispersion. The rpm experimentation range was chosen based on a
series of preliminary tests where the desired flowability of the mixture measured by the micro-cone
spread test and the required water-to-solids ratio were taken into consideration. Tests showed that
the rpm of the mixer should be preferably among 3000–5000. For the chosen mixing time, more than
5000 rpm results in less workable mixtures due to the increased number of revolutions [32].
Subsequently, after the range of the proportions of the ingredients in the mixtures was estimated,
the Box–Behnken fractional factorial design of experiments was used to estimate the effect of synthesis
parameters and mixing speed on the properties of the produced CMC [8,33]. Factorial design of
experiments allows an experimenter to make intentional changes to the design parameters (also called
factors) of a process in order to identify and observe the changes that occur to the response variables.
In this study, four factors were considered:

- Cement and fly ash to quarry dust ratio (CFA/D);

- Aerating agent to cement and fly ash ratio (Al/CFA);
- Superplasticizer (wt%) (SPL);
- Revolutions per minute (rpm) of the mixer (RPM).

Following the standard notation used in factorial design, the above factors were also coded as A,
B, C, and D, respectively.
The examined response variables included the water-to-solids ratio (w/s) of the fresh mixture and
the compressive strength (Fc ), flexural strength (Ff ), density (d), water absorption (Wa ), and thermal
conductivity (λ) of hardened specimens.
Each design parameter was tested at three levels, low, medium, and high, coded as −1, 0, 1,
respectively. The selected levels of design parameters are given in Table 2.
A full factorial experimental design of 4 factors with 3 levels of experimentation would result in
4
81 (3 ) mixtures, while a Box–Behken fractional design using a subset of a full factorial design leads to
25 mixtures. For the calculation of the measurement error, the middle level (0) is repeated three times.
Thus, a total of 27 mixtures were finally prepared and tested. The resulting combinations are shown
in Table 2. Table 2 also contains the design parameters of a reference mixture which was prepared
without the addition of aerating agent.
Box–Behnken design allows the development of an adequate model relating a response variable
y and the associated k design parameters denoted by x1 , x2 , . . . , xk by using the response surface
methodology. The developed model can be used to find optimum settings of xi that result in
the maximum or minimum response y over a region of interest. Box–Behnken factorial design of
experiments uses three levels of experimentation for each design parameter and requires significantly
smaller number of experiments compared to full factorial design of experiments. It is widely used
for the development of second order polynomial models for relating a response variable y and the
associated design parameters xi [33,34].

k
X X k
X
y = b0 + bi xi + bij xi x j + bii x2i + ε (2)
i=1 i,j i=1

where b0 is the constant term, bi and bii are the first and second order coefficients, respectively, bij are
the coefficients for the interactions xi xj , and ε is the prediction error.
Buildings 2020, 10, 214 7 of 17

Table 2. Parameters and levels of design, mixtures prepared according to Box–Behnken factorial design,
and raw material proportions.

Design Parameters * Raw Materials Proportions (kg/m3 )

Mixture
No. Fly CEM I Quarry Aerating
A B C D Superplasticizer Water
Ash 42.5N Dust Agent
1 0.430 0.075 0.000 4000 140 210 817 26 0.00 370
2 0.715 0.075 0.125 4000 173 255 592 32 1.32 379
3 1.000 0.075 0.125 3000 195 293 489 37 1.27 422
4 0.715 0.075 0.125 4000 173 255 592 32 1.32 379
5 0.715 0.050 0.125 5000 174 256 593 21 1.31 388
6 0.430 0.075 0.125 3000 126 190 737 24 1.35 351
7 0.715 0.050 0.000 4000 196 288 667 24 0.00 388
8 0.715 0.075 0.125 4000 173 255 592 32 1.32 379
9 0.715 0.100 0.125 3000 173 254 590 43 1.33 370
10 1.000 0.075 0.000 4000 218 327 546 41 0.00 430
11 1.000 0.075 0.250 4000 184 276 460 34 2.39 370
12 0.430 0.075 0.250 4000 117 176 685 22 2.50 313
13 0.430 0.100 0.125 4000 125 188 732 31 1.35 351
14 0.715 0.075 0.250 5000 158 233 541 29 2.40 361
15 0.430 0.050 0.125 4000 127 191 743 16 1.35 351
16 0.715 0.100 0.250 4000 161 236 548 40 2.46 332
17 0.715 0.100 0.125 5000 172 252 586 42 1.32 379
18 1.000 0.050 0.125 4000 199 299 498 25 1.28 414
19 1.000 0.075 0.125 5000 200 300 500 37 1.30 396
20 0.715 0.050 0.250 4000 164 241 559 20 2.46 332
21 0.715 0.075 0.000 3000 194 285 661 36 0.00 388
22 0.715 0.100 0.000 4000 187 276 640 46 0.00 414
23 0.715 0.050 0.125 3000 171 252 584 21 1.29 405
24 0.715 0.075 0.250 3000 161 237 549 30 2.44 342
25 0.715 0.075 0.000 5000 195 287 666 36 0.00 379
26 0.430 0.075 0.125 5000 124 187 726 23 1.33 370
27 1.000 0.100 0.125 4000 196 294 490 49 1.29 405
Reference 0.715 0.000 0.125 4000 175 257 597 0 1.29 405
* Levels of design: Low (−1) Medium (0) High (+1)
CFA/D (A): Cement and fly ash to quarry dust ratio 0.430 0.715 1.000
Al/CFA (B): Aerating agent to cement and fly ash ratio 0.050 0.075 0.100
SPL (C): Superplasticizer (wt%) 0.000 0.125 0.250
RPM (D): Revolutions per minute (rpm) of the mixer 3000 4000 5000

2.4. Specimen Preparation and Testing

Quarry dust was dry mixed with cement, fly ash, superplasticizer, and aerating agent. Then,
water was added to the dry mixture gradually until the mixture obtained the required flowability
measured by the micro-cone spread test, and water-to-solids ratio was calculated. The micro-cone
spread test is a modified version of the flow cone test EN 11041, which measures the flowability
of fresh micro-concrete [31]. Micro-cone spread diameter was calculated as a mean value of three
micro-cone spread measurements regarding the reference mixture and was used as a reference value
for the produced mixtures. The measured spread cone diameter was 12.7 cm. Accepted micro-cone
spread test values ranged between 12 and 13 cm. Mixture proportions are indicated in Table 2.
Following mixing procedure, fresh mixture was poured into prismatic molds (4 × 4 × 16 cm3 ) and
was left for 24 h to expand, to form its cellular structure, and to achieve the hardening required for the
demolding (Figure 6a,b). The produced specimens were then cured for 28 days in a Matest E139 curing
chamber (at 20 ± 2 ◦ C and a relative humidity of at least 95%) according to EN 196-1.
 test values ranged between 12 and 13 cm. Mixture proportions are indicated in Table 2.
Following mixing procedure, fresh mixture was poured into prismatic molds (4 × 4 × 16 cm3) and
was left for 24 h to expand, to form its cellular structure, and to achieve the hardening required for
the demolding (Figure 6a,b). The produced specimens were then cured for 28 days in a Matest E139
curing 2020,
Buildings chamber
10, 214(at 20 ± 2 °C and a relative humidity of at least 95%) according to ΕΝ 196-1. 8 of 17

(a) (b)
Figure 6.
Figure 6. (a)
(a)Mixtures
Mixturescast into
cast 40 ×4040××40
into 160×mm
160 molds
3 after aeration;
mm3 molds (b) specimen
after aeration; with flattened
(b) specimen with
surface.
flattened surface.

Foreach
For eachhardened
hardened specimen,
specimen, the compressive
the compressive and flexural
and flexural strength,strength, dry
dry density, density,
water water
absorption,
absorption,
and thermal and thermal conductivity
conductivity were measured.were measured.
Measurementofofcompressive
Measurement compressive(F(Fc andflexural
)c)and flexural(F(Ff )f)strength
strengthwas
wasperformed
performedaccording
accordingtotoEN EN196-1
196-
1 using
using a Matest
a Matest E161-03N
E161-03N compressionand
compression andflexural
flexuralmachine
machinewithwithdual
dualrange
range500/15
500/15kN.
kN.For For each
each
mixture,33specimens
mixture, specimenswere wereproduced
producedand andtested,
tested,and
andcompressive
compressiveand andflexural
flexuralstrength
strengthvalues
valueswere
were
calculatedas
calculated astheir
theiraverage.
average.
Determinationof
Determination ofthermal
thermalconductivity
conductivityof ofspecimens
specimens(λ) (λ)was
wasconducted
conductedaccording
accordingtotoradial
radialheat
heat
flowmethod
flow method[35].[35]. This
This method
method uses
uses thermocouples
thermocouples to to measure
measure temperature
temperature difference
difference at
at aaspecific
specific
distancewhen
distance whenheatheatQ 𝑄 flows
flows through
through aa sample.
sample. More
More specifically,
specifically,aacylindrical
cylindricalsample
sampleisisheated
heatedat atthe
the
axisand
axis andthetheheat
heatflows
flowsradially
radiallyoutwards,
outwards,as asseen
seenininFigure
Figure7.7. The
The thermal
thermal conductivity
conductivity isis given
given byby
Equation(3):
Equation (3):
r
Q ln( r21 )r
λ = Q ln( 2 ) (3)
2πh∆T r (3)
where r1 and r2 refer to the distance between λthe= two thermocouples and the axis of the sample, h is
1

Buildings 2020, 10, x FOR PEER REVIEW 2π hΔT 9 of 18

the height of the sample, and ∆T is the temperature difference between the two thermocouples [35].
where r1 and r2 refer to the distance between the two thermocouples and the axis of the sample, h is
the height of the sample, and ΔT is the temperature difference between the two thermocouples [35].
The measured cylindrical samples in this study were extracted from the hardened prismatic
specimens using a diamond core drilling tool. The sample diameter was 35 mm, the height h was 40
mm, and the distances between the two thermocouples and the axis of the sample r1 and r2 were 8
and 12 mm, respectively. Thermal conductivity measurements were conducted under stable ambient
conditions at 21 ± 1°C.

(a) (b)
Figure 7.
Figure 7. (a) Experimental setup for the measurement
measurement of
of thermal
thermal conductivity;
conductivity; (b)
(b) schematic
schematic of
of radial
radial
heat flow method. Based on Zhao et al.
heat flow method. Based on Zhao et al. [35].[35].

The measured
3. Analysis cylindrical
of Results samples in this study were extracted from the hardened prismatic
and Discussion
specimens using a diamond core drilling tool. The sample diameter was 35 mm, the height h was
The results of factorial design are given in Table 3 and show the mixtures’ design parameters
40 mm, and the distances between the two thermocouples and the axis of the sample r1 and r2 were
(A, B, C, D) along with the selected response variables (w/s, d, Fc, Ff, Wa, and λ). The density d of the
8 and 12 mm, respectively. Thermal conductivity measurements were conducted under stable ambient
hardened specimens varies from 680 to 1080 kg/m3 and is considerably lower compared to the
conditions at 21 ± 1 ◦ C.
reference (1530 kg/m3) that was prepared without the addition of the aerating agent. This decrease in
density affected physical and mechanical properties of the produced cellular micro-concrete (CMC)
significantly.
In order to determine the effect of synthesis parameters on the properties of the produced CMC
specimens and to optimize mixture composition, results analysis was conducted in two stages.
Firstly, measured physical and mechanical properties of fresh and hardened CMC specimens were
correlated with density and compared to reference values, and secondly, the factorial
experimentation was analyzed, and the modeling and optimization were performed.
Buildings 2020, 10, 214 9 of 17

3. Analysis of Results and Discussion

The results of factorial design are given in Table 3 and show the mixtures’ design parameters (A,
B, C, D) along with the selected response variables (w/s, d, Fc , Ff , Wa , and λ). The density d of the
hardened specimens varies from 680 to 1080 kg/m3 and is considerably lower compared to the reference
(1530 kg/m3 ) that was prepared without the addition of the aerating agent. This decrease in density
affected physical and mechanical properties of the produced cellular micro-concrete (CMC) significantly.

Table 3. Box–Behnken factorial design and test results.

Design Parameters Response Variables

Mixture
No. d Fc Ff λ Wa
A B C D w/s
(kg/m3 ) (MPa) (MPa) (W/m·K) (%)
1 0.430 0.075 0.000 4000 0.31 780 2.8 2.6 0.20 37.2
2 0.715 0.075 0.125 4000 0.32 870 3.9 3.3 0.24 32.3
3 1.000 0.075 0.125 3000 0.37 770 4.3 2.6 0.24 37.3
4 0.715 0.075 0.125 4000 0.32 900 4.0 3.4 0.25 31.1
5 0.715 0.05 0.125 5000 0.33 950 5.3 3.5 0.30 30.1
6 0.430 0.075 0.125 3000 0.29 920 4.3 3.2 0.27 30.7
7 0.715 0.050 0.000 4000 0.33 890 3.8 3.1 0.24 32.2
8 0.715 0.075 0.125 4000 0.32 910 4.7 3.4 0.29 31.4
9 0.715 0.100 0.125 3000 0.31 900 4.2 3.3 0.28 30.3
10 1.000 0.075 0.000 4000 0.38 690 2.4 1.9 0.18 45.1
11 1.000 0.075 0.250 4000 0.31 900 6.4 3.4 0.28 31.9
12 0.430 0.075 0.250 4000 0.25 930 5.5 3.3 0.28 30.4
13 0.430 0.100 0.125 4000 0.29 930 3.4 3.0 0.25 30.6
14 0.715 0.075 0.250 5000 0.30 860 6.1 3.8 0.24 33.8
15 0.430 0.050 0.125 4000 0.29 1030 6.3 3.4 0.33 26.3
16 0.715 0.100 0.250 4000 0.27 970 6.3 4.2 0.28 28.5
17 0.715 0.100 0.125 5000 0.32 860 4.9 3.3 0.23 34.2
18 1.000 0.050 0.125 4000 0.36 810 4.3 2.7 0.22 34.8
19 1.000 0.075 0.125 5000 0.34 860 6.7 2.8 0.23 33.5
20 0.715 0.050 0.250 4000 0.27 1080 7.1 5.6 0.31 23.8
21 0.715 0.075 0.000 3000 0.33 830 3.3 2.5 0.25 34.1
22 0.715 0.100 0.000 4000 0.36 680 1.9 1.9 0.19 40.1
23 0.715 0.050 0.125 3000 0.35 880 5.3 3.5 0.28 33.6
24 0.715 0.075 0.250 3000 0.28 850 5.0 3.5 0.27 30.2
25 0.715 0.075 0.000 5000 0.32 720 2.5 4.4 0.19 41.3
26 0.430 0.075 0.125 5000 0.31 900 4.5 3.2 0.24 32.8
27 1.000 0.100 0.125 4000 0.35 790 3.6 2.7 0.22 36.2
Reference 0.715 0.000 0.125 4000 0.35 1530 25.8 7.4 0.49 18.1

In order to determine the effect of synthesis parameters on the properties of the produced CMC
specimens and to optimize mixture composition, results analysis was conducted in two stages. Firstly,
measured physical and mechanical properties of fresh and hardened CMC specimens were correlated
with density and compared to reference values, and secondly, the factorial experimentation was
analyzed, and the modeling and optimization were performed.
Moreover, the physical and mechanical properties of the produced cellular micro-concrete were
compared to those obtained by other researchers in previous studies [36–39].

3.1. Correlation of Measured Properties

Results of Table 3 indicate that the measured response variables (d, Fc , Ff , Wa , λ and w/s) for
the hardened specimens are not independent but showed strong correlation. Figure 8 presents
the correlation diagram between the measured response variables, while Table 4 gives the Pearson
correlation coefficients for each pair of response variables. These correlation coefficients range between
−1 and +1 and measure the strength of the linear relationship between the variables. From Figure 8
variable.
It is well known that density is related to the pore structure of CMC. Any change in the pore
structure of CMC may influence the material properties significantly in relation to density. More
specifically, an increase in the porosity of CMC results in lower density, which in turn decreases the
mechanical strength, while thermal insulation is enhanced [40,41]. Analysis of the CMC pore
Buildings 2020, 10, 214 10 of 17
structure was beyond the scope of this study. However, since porosity and density are highly
correlated (as shown in Table 4 and Figure 8), density is considered as the characteristic physical
property
and Tableof4,produced CMC
it can be seen specimens
that which
d, Fc , Ff , W largely
a , λ, and w/s determines
are stronglyall the otherDensity
correlated. examined response
(d) shows the
variables.
higher correlation coefficients and can be considered as the most decisive response variable.

d
Fc
Ff
Wa
λ
w/s
Correlationdiagram
Figure8.8.Correlation
Figure diagrambetween
betweenresponse
responsevariables
variables(d,
(d,FFc,c ,FFf,f W
,W , λ,and
a,aλ, andw/s).
w/s).

Table 4. Pearson correlation coefficients for each pair of response variables (d, Fc , Ff , Wa , λ, and w/s).
Table 4. Pearson correlation coefficients for each pair of response variables (d, Fc, Ff, Wa, λ, and w/s).
d Fc F Wa λ w/s
d Fc Ff f Wa λ w/s
d 1.00 d 1.00
0.80 0.80 0.870.87 −0.96
−0.96 0.93 −0.70
0.93 −0.70
F 0.80 1.00 0.84 −0.75 0.67 −0.55
Fc 0.80 c 1.00 0.84 −0.75 0.67 −0.55
Ff 0.87 0.84 1.00 −0.86 −0.83 −0.65
Ff 0.87 Wa 0.84
−0.96 −0.75 1.00−0.86 −0.86 −0.91
1.00 −0.83
0.73 −0.65
Wa −0.96 λ −0.75
0.93 0.67 −0.86 0.83 1.00 1.00
−0.91 −0.91
−0.79 0.73
λ 0.93 w/s −0.70
0.67 −0.55 0.83−0.65 −0.91 −0.79
0.73 1.00
1.00 −0.79
w/s −0.70 −0.55 −0.65 0.73 −0.79 1.00
It is well known that density is related to the pore structure of CMC. Any change in the
3.2. Physical and Mechanical
pore structure of CMC may Properties of Produced
influence CMC Compared
the material propertiestosignificantly
Reference Mixture
in relation to density.
More specifically, an increase in the porosity of CMC results in lower density, which in turn decreases
the mechanical strength, while thermal insulation is enhanced [40,41]. Analysis of the CMC pore
structure was beyond the scope of this study. However, since porosity and density are highly correlated
(as shown in Table 4 and Figure 8), density is considered as the characteristic physical property of
produced CMC specimens which largely determines all the other examined response variables.

3.2. Physical and Mechanical Properties of Produced CMC Compared to Reference Mixture
Figure 9 presents the percentage change in Fc , Ff , d, Wa , and λ for the three levels of aerating
agent to cement and fly ash ratio (0.05, 0.075, and 0.1) compared to the reference mixture (no aerating
agent addition). Percentage change in the response variables was chosen to be examined in relation
to the aerating agent to cement and fly ash ratio since this ratio determines the degree of aeration.
In this way, the aerating agent to cement and fly ash ratio has a significant effect on the density of the
hardened specimens, which is a physical property of great importance since, as already mentioned
above, it strongly affects all the measured properties.
As seen in Figure 9a, the decrease rate of Fc compared to that of Ff , for the same d decrement,
is significantly higher. More specifically, a decrease in d of around 39% causes an Fc decrease of 80%,
whereas Ff decreases by around 51%, for an aerating agent to cement and fly ash ratio of 0.05. Figure 9b
shows that the decrement of d causes a significant increase in Wa . More specifically, a 50% decrease in
d provokes a Wa increase of 89%, for an aerating agent to cement and fly ash ratio of 0.075. On the
other hand, it seems that the decrease rate of d is similar to that of λ.
Buildings 2020, 10, 214 11 of 17

From Figure 9a,b, it can be observed that the increase in aerating agent to cement and fly ash
ratio from 0.075 to 0.1 does not cause any significant change in the measured properties. This can be
attributed to the fact that the mixtures produced with higher aerating agent to cement and fly ash ratio
have insufficient amounts of CaO, which is related to the cement and fly ash content of the mixture.
In this way, the produced mixtures do not have the required amount of CaO to react with the higher
Buildings 2020, 10, x FOR PEER REVIEW 13 of 19
amount of aluminum powder and provoke further aeration.

(a)

(b)
Figure9.9. Percentage change
Figure change inin(a)
(a)FFc,cF
, fF, fand
, andd; d;
(b)(b)
d, W , and
d, aW λ, for
a , and λ, the
for three levels
the three of aerating
levels agent
of aerating
to cement and fly ash ratio (0.05, 0.075, and 0.1) compared to the reference mixture
agent to cement and fly ash ratio (0.05, 0.075, and 0.1) compared to the reference mixture (no aerating (no aerating agent
addition).
agent addition).

3.3.
3.3.Factorial
FactorialDesign
DesignAnalysis,
Analysis,Modeling,
Modeling,and
andOptimization
Optimization
The
TheBox–Behnken
Box–Behnkenfactorial factorialdesign
designresults
resultswere
wereanalyzed
analyzedaccording
accordingto tothe
thestandard
standardmethodology
methodology
proposed
proposed by Myers and Montgomery [33]. The conducted analysis included thecalculation
by Myers and Montgomery [33]. The conducted analysis included the calculationof ofmain
main
effects (first and second order) and interactions of design parameters (A, B, C,
effects (first and second order) and interactions of design parameters (A, B, C, and D) on the response and D) on the response
variables
variables(F (Fcc,, FFff,, d,
d, WWaa, ,λ,λ,and
andw/s)
w/s)ininorder
ordertotoidentify
identifythose
those which
which have
have a significant
a significant effect
effect on on
the
the response.
response.
The
Thefirst
firstorder
ordermain main effect (factor)
effect of of
(factor) a design
a designparameter
parameteron aonresponse
a responsevariable is estimated
variable as the
is estimated as
difference between the response of a factor at the high level and at the low level,
the difference between the response of a factor at the high level and at the low level, when all other when all other factors
are adjusted
factors at their central
are adjusted at their values (midway
central valuesbetween
(midway their low and
between high
their lowlevels). The interactions
and high levels). The
between two factors express the additional effect of one factor, when
interactions between two factors express the additional effect of one factor, when the other the other one is held at itsone
highis
level. Interactions occur when the effect of one factor is different at various levels
held at its high level. Interactions occur when the effect of one factor is different at various levels of of the other factor.
Second
the otherorder
factor.effects express
Second orderthe quadratic
effects express relationship
the quadraticbetween designbetween
relationship parametersdesignandparameters
response
variables [42,43].
and response variables [42,43].
Next,
Next,the theestimated
estimatedeffects effectswere
weredivided
dividedby bythe
themeasurement
measurementerror errortotoobtain
obtainthethestandardized
standardized
values.
values. Standardized values, whose absolute value exceeded 1.96, were regarded asstatistically
Standardized values, whose absolute value exceeded 1.96, were regarded as statistically
significant. This value (1.96) results from the normal distribution at confidence level 95%. After this,
the statistically significant factors were used to develop second order polynomial models linking
response variable with factors. Finally, the identification of the optimal design parameters was
performed by using the response surface methodology. The above analysis was carried out by using
the STATGRAPHICS 5 Plus software package version 15.2.11 (StatPoint Technologies, Inc.,
Buildings 2020, 10, 214 12 of 17

significant. This value (1.96) results from the normal distribution at confidence level 95%. After this,
the statistically significant factors were used to develop second order polynomial models linking
response variable with factors. Finally, the identification of the optimal design parameters was
performed by using the response surface methodology. The above analysis was carried out by using
the STATGRAPHICS 5 Plus software package version 15.2.11 (StatPoint Technologies, Inc., Warrenton,
VA, USA).
The standardized estimated values of main effects, interactions, and second order effects of design
factors on the response variables are given in Table 5. Al/CFA factor has the strongest effect on all
response variables compared to other design factors. The increase in Al/CFA reduces greatly d, Fc ,
Ff , and λ (negative effect) and increases significantly Wa (positive effect). CFA/D has a similar effect
with Al/CFA on d, Fc , Ff , Wa and λ; however, its magnitude is considerably lower. On the other hand,
the increase in CFA/D increases w/s. SPL has the opposite effect on d, Fc , Ff , Wa , and λ compared to
CFA/D and Al/CFA. With regard to w/s, an increase in SPL causes its countable reduction. Finally,
the main effects of RPM on response variables are low and statistically significant only for d, w/s,
and Wa . Several interactions and second order effects also appear statistically significant for all response
variables, indicating the non-linear relationship between design factors and response variables.

Table 5. Standardized values of main effects, interactions, and second order effects of design factors on
the response variables.

Main Effects of Design Factors Interactions Second Order Effects

Response
Variable A B C D
A×B A×C A×D B×C B×D C×D A2 B2 C2 D2
CFA/D Al/CFA SPL RPM
d −8.92 −37.03 6.86 3.24 4.71 1.76 3.24 5.88 −6.47 3.53 −2.12 26.18 −4.04 −2.27
Fc −4.03 −67.32 8.93 −0.14 7.30 1.98 1.03 3.90 2.37 3.27 1.41 54.61 1.71 2.89
Ff −6.42 −39.98 17.27 0.18 4.30 4.40 1.05 −1.50 −0.20 3.90 −8.25 27.72 −1.07 −2.62
Wa 13.18 27.90 −13.91 −4.28 −5.90 −6.41 −5.86 −6.44 14.88 −3.59 7.54 −15.83 8.44 5.06
λ −9.33 −21.88 5.17 1.17 8.00 0.01 1.00 2.00 −4.00 1.50 −0.55 17.87 −0.80 −2.30
w/s 20.56 −9.37 −13.37 −5.14 −3.08 −1.54 −7.71 −9.25 9.25 4.63 2.51 6.04 −8.29 2.51

The statistically significant factors were selected to develop second order polynomial models
linking response variables with factors. The developed models are given in Equations (4)–(9).

d = 1083.33 − 374.27A − 8407.02B − 253.333C + 0.18D − 292.40A2 + 2807.02AB + 0.10AD +

(4)
54000.00B2 + 8000.00BC − 1.1BD − 2560.0C2 + 0.24CD − 0.000025D2 (R = 0.91)

Fc = 20.77 − 7.01A − 220.91B − 15.62C − 0.0025D + 76.84AB + 8.35AC + 684.67B2 + 93.6BC

(5)
+ 0.0065BD + 0.0039CD + 2.05 × 10−7 D2 (R = 0.96)

Ff = 4.81 + 4.33A − 107.60B − 4.05C + 0.00073D − 4.88A2 + 15.09AB + 6.18AC + 564.25B2 +

(6)
0.0016CD − 1.15 × 10−7 D2 (R = 0.96)

Wa = 38.74 + 9.73A + 106.35B + 12.18C − 0.01D + 23.21A2 − 103.51AB − 44.98AC −

0.0051AD −1582.60B2 − 257.6BC + 0.074BD + 135.08C2 − 0.0072CD + 0.0000013D2 (7)
(R = 0.95)

λ = 0.48 − 0.30A − 7.2B + 0.13C + 0.000091D + 2.81AB + 36.71B2 + 1.60BC − 0.00023BD −

(8)
9.97 × 10−9 D2 (R = 0.97)

w/s = 0.310722 + 0.252693A − 1.04912B − 0.0231579C − 0.0000294737D + 0.0461681A2 −

0.350877AB − 0.0701754AC − 0.0000438596AD + 2.0B2 − 2.4BC + 0.0003BD − 0.88C2 (9)
+ 0.00006CD +3.75 × 10−9 D2 (R = 0.90)
The estimated regression coefficients R for the models (4) to (9) varied between 0.90 and 0.97,
indicating that there is a reasonable agreement between predicted and observed values. Thus, the fitted
polynomial models describe adequately the influence of the design factors on response variables
Buildings 2020, 10, 214 13 of 17

and can be used successfully for the prediction of CMC properties. However, it must be stated
that these regression models are accurate and reliable only when the design factors are within the
experimentation range.
Figure 10 shows the response surface of density, compressive strength, and water absorption as a
function of Al/CFA and CFA/D. SPL and RPM were kept constant at their middle levels. Density and
compressive strength indicate similar response surfaces, since they a have strong positive correlation.
In contrast, the response surface for water absorption is reversed, since density and water absorption
Buildings 2020, 10,negative
have a strong x FOR PEER REVIEW
correlation. 15 of 19

Estimated Response Surface

SPL=0.125 wt%, RPM=4000 d (kg/m^3)
700.0
800.0
1590 900.0
1000.0
1390
d (kg/m^3)

1100.0
1190 1200.0
990 1300.0
0.12 1400.0
790 0.08
0.04 1500.0
0.43 0.53 0.63 0.73
0.83 0.93 1.03 0 Al/CFA 1600.0
CFA/D

(a)

Estimated Response Surface

SPL=0.125 wt%, RPM=4000

Fc (MPa)
13.4 0.0
2.0
11.4
4.0
Fc (MPa)

9.4 6.0
7.4 8.0
5.4 0.12 10.0
3.4 0.08 12.0
0.43 0.53 0.63 0.73 0.04
0.83 0.93 1.03 0 Al/CFA
CFA/D

(b)

Estimated Response Surface

SPL=0.125 wt%, RPM=4000
Wa (%)
10.0
40 15.0
35 20.0
30 25.0
Wa (%)

25 30.0
20 35.0
15 0.12 40.0
10 0.08
0.43 0.53 0.63 0.73 0.04
0.83 0.93 1.03 0 Al/CFA
CFA/D

(c)
Figure
Figure 10.
10. Plots
Plotsofofresponse
responsesurfaces
surfacesofof(a)(a)density;
density;(b)(b)
compressive strength;
compressive (c)(c)
strength; water absorption,
water as
absorption,
function ofof
as function the
thedesign
designfactors CFA/Dand
factors CFA/D andAl/CFA.
Al/CFA.SPLSPLandand
RPMRPM are kept
are kept constant
constant atmiddle
at their their middle
levels.
levels.

Polynomial models developed above (4)–(9) allow the design of mixtures with predefined
and/or optimized values of physical and mechanical properties of the produced CMC by using the
multiple response optimization method developed by Myers and Montgomery, [33].
In this study, three different optimization cases were examined. In the first and second case, the
goal of the optimization was to maximize the compressive strength for predefined values for density
Buildings 2020, 10, 214 14 of 17

Polynomial models developed above (4)–(9) allow the design of mixtures with predefined and/or
optimized values of physical and mechanical properties of the produced CMC by using the multiple
response optimization method developed by Myers and Montgomery, [33].
In this study, three different optimization cases were examined. In the first and second case,
the goal of the optimization was to maximize the compressive strength for predefined values for
density (d = 700 kg/m3 and d = 800 kg/m3 ). In the third case, the goal was to minimize density and to
maximize compressive strength simultaneously. Based on the optimum design factors corresponding
to each optimization case, CMC specimens were produced and tested for their compressive strength
and density. The optimization results are given in Table 6. As seen in Table 6, measured values validate
the design methodology since the differences between designed and measured values are in the range
of measurement error (0.5 MPa for Fc and 17 kg/m3 for d).

Table 6. Optimization results.

Optimization Optimum Values for Factors Predicted Measured

No.
Goal CFA/D Al/CFA SPL RPM d (kg/m3 ) Fc (MPa) d (kg/m3 ) Fc (MPa)
d = 700 kg/m3 &
1 1.000 0.057 0.000 3000 700 3.4 715 3.8
Fc = max
d = 800 kg/m3 &
2 1.000 0.042 0.076 3000 800 4.9 810 5.2
Fc = max
d = min &
3 1.000 0.036 0.250 3000 813 6.6 830 7.1
Fc = max

3.4. Comparison with Previous Studies

For the comparison of the properties of the produced cellular micro-concrete specimens with
those obtained in previous studies, the strength-to-density ratio (Fc /d) was used. Table 7 shows the
Fc /d obtained in this study and those derived from other selected studies regarding the production of
moist-cured cellular concrete (20 ± 2 ◦ C and at least 90% relative humidity for 28 days), with density
values ranging between 400 and 1300 kg/m3 . As seen in Table 7, research studies regarding the
production of moist-cured cellular concrete using aluminum powder as an aerating agent are limited.

Table 7. Comparison of compressive strength-to-density ratio (Fc /d) for moist-cured cellular concrete.

Compressive
Aerating Strength-to-Density Density
Raw Materials Reference
Agent Ratio, Fc /d (kg/m3 )
([MPa/(kg/m3 )] × 10−3 )
Clayey fines
Aluminum
(kaolinites), CEM I 1.1–3.7 850–1050 Goual et al. [36]
powder
52.5N
River sand,
Aluminum Kumar and
Portland Pozzolana 0.6–8.3 450–1250
powder Ramamurthy [37]
Cement (PPC)
Quarry dust, Sodium lauryl
9.0–10.3 800–1200 Tharakarama et al. [38]
CEM I 52.5N sulphate
River sand,
siliceous fly ash,
gypsum, Protein-based
1.0–1.4 920–1130 Oren et al. [39]
granulated blast agent
furnace slag,
CEM II 42.5R
Quarry dust,
Aluminum
calcareous fly ash, 2.8–6.5 680–1080 Present study
powder
CEM I 42.5N
Buildings 2020, 10, 214 15 of 17

In this study, the acquired Fc /d and density values of cellular concrete produced with quarry dust,
calcareous fly ash, CEM I 42.5N, and aluminum powder as an aerating agent, ranged between 2.8 and
6.5 ([MPa/(kg/m3 )] × 10−3 ) and 680–1080 kg/m3 , respectively.
Based on Fc /d ratio, the moist-cured cellular concrete prepared in this study outperforms most of
those presented in Table 7. There are some cases where Fc /d ratio exceeds the one calculated in this
study; however, it must be noted that, in these cases, the examined cellular concrete products had
density values as high as 1200–1250 kg/m3 , while in parallel, a high-strength cement (CEM I 52.5N)
was used for their preparation.

4. Conclusions
The factorial design results indicated that the aerating agent to cement and fly ash ratio has a
significant effect on the density of the hardened specimens, which is a physical property of great
importance since it strongly affects all the measured properties (compressive and flexural strength,
water absorption, and thermal conductivity). Moreover, the results showed that cement and fly ash
to quarry dust ratio has a similar effect with aerating agent to cement and fly ash ratio on response
variables. Superplasticizer dosage has the opposite effect on response variables compared to aerating
agent to cement and fly ash ratio and cement and fly ash to quarry dust ratio, whereas the effect of
mixer speed (revolutions per minute) on response variables is low and statistically significant only for
density, water absorption, and water-to-solids ratio.
The developed polynomial models describe adequately the non-linear influence of the design
factors on response variables and can be used successfully for the prediction of cellular micro-concrete
properties; however, the developed regression models are accurate and reliable only when the
design factors are within the experimentation range. In this way, regarding the optimization results,
the measured values validated the design methodology. Since factorial design of experiments and
the response surface methodology have been successfully used for product design and improvement
in several industrial applications, we consider that the proposed mixture design methodology
could be used at industrial scale. However, with regard to the required long curing time,
industrial-scale applications would demand large CMC curing installations and additional costs.
However, the additional costs could be compensated by the lower energy required (compared to
energy-intensive hydrothermal curing process).
Concerning the comparison between the existing studies and the current study, it should be
mentioned that the prepared cellular micro-concrete, which utilizes a large amount of quarry dust
(around 50% to 70%), outperforms most of the examined similar cellular concrete products.
Finally, besides CMC conventional moist-curing, the production of low-density CMC using rapid
curing techniques in a CO2 environment so as to accelerate hardening, improve physical-mechanical
properties, and mitigate the environmental impact is under investigation for possible applications.

Author Contributions: Conceptualization, M.G.; Formal analysis, A.S. and M.G.; Investigation, A.S.; Methodology,
M.G.; Supervision, M.G.; Writing–original draft, A.S.; Writing–review & editing, M.G. All authors have read and
agreed to the published version of the manuscript.
Funding: This research received no external funding.
Acknowledgments: This work was performed under the framework of the project “National Contribution to
European competitive projects—BEWEXMIN” (82287) managed by the Research Committee of the Technical
University of Crete.
Conflicts of Interest: The authors declare no conflict of interest.

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