Construction and Building Materials 350 (2022) 128921

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Construction and Building Materials

journal homepage: www.elsevier.com/locate/conbuildmat

Microstructure characterizations, thermal analysis, and compression

stress–strain behavior of lime-based plaster
Chiya Y. Rahimzadeh a, b, *, Ahmed Salih Mohammed c, *, Azeez A. Barzinjy d, e
a
Scientific Research Centre, Soran University, Soran, Kurdistan-Region, Iraq
b
Civil Engineering Department, Faculty of Engineering, Soran University, Soran, Kurdistan-Region, Iraq
c
Civil Engineering Department, College of Engineering, University of Sulaimani, Kurdistan, Iraq
d
Department of Physics, Salahaddin University-Erbil, Erbil, Kurdistan-Region, Iraq
e
Department of Physics Education, Faculty of Education, Tishk International University, Erbil, Kurdistan-Region, Iraq

A R T I C L E I N F O A B S T R A C T

Keywords: Classical lime-based plasters (LP) are multilayer complex systems made of different fillers and binders; the
Lime-based plaster (LP) behavior of LPs is determined by their physical properties: mutual connection, contact with the substrates, and
Microstructure tests external factors. Lime plaster is set to a solid mass that is durable and relatively flexible. It is permeable and
Stress–strain
allows for moisture diffusion and evaporation. It is less affected by water and will not dry or dissolve like clay or
Curing time
gypsum plaster. Plasters of hydrated lime are less brittle and less prone to breakage, which do not require
Modeling
expansion joints. Different plasters have been used in construction industries, such as cement, lime, mud, stucco,
and gypsum plasters. Lime-based plaster (LP) is used as building insulation materials (Bims) against environ­
mental impacts. Lime plaster is made of sand, water, and lime, usually non-hydraulic hydrated lime (also known
as slaked lime, high calcium lime, or air lime). Ancient lime plaster often contained horse hair for reinforcement
and pozzolanic additives to reduce work time. Microstructure tests such as X-ray fluorescence (XRF), energy
dispersive X-ray (EDX), X-ray diffraction, scanning electron microscopy, and differential scanning calorimetry
were used to identify the LP. Thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy,
compressive strength, and modulus of elasticity. The XRF and EDX study revealed that the LP was mainly
composed of SiO2 and CaO, predominantly changed into calcium-silicate and CaCO3 throughout the carbonation
process. TGA results showed that the LP had high thermal stability up to 150 ◦ C and 16.6 % weight loss at
1000 ◦ C, proving the significant heat capacity of the material and fire resistance.
The compressive strength of the LP with water to binder ratio (w/b) of 0.75 and 0.9 were 900 and 350 kPa at
28 days of curing, respectively. Three distinct mathematical models, including β, rational, and Vipulanandan p-q
models, were proposed to predict stress–strain relationships of the LP. Based on the statistical parameters such as
coefficient of determination (R2), root mean square error (RMSE), and mean absolute error (MAE), the Vipu­
lanandan p-q model was the best model for predicting the stress–strain behavior of the LP.

1. Introduction base for paint, distempering, whitewashing, or shading. It shields the

Conventional lime-based plasters (LP) are exceedingly sophisticated
structures made of many binders; their behavior is determined by their
physical properties, connection to one another, interaction with the
wall, floor, roof substrate surfaces, and other outside influences.
The Cement Plaster of the inside and outside wall house is a significant
undertaking as it delivers an ideal completion to the wall surface and
adds solidarity to them. A layer of plaster can disguise lopsided surfaces,
making your walls look even, smooth, and clean. Plastering gives a good
walls from downpours and other natural factors that could harm the
design. Plaster is applied to substantial workmanship surfaces in a few
coats comprising basecoat(s) and a completion coat. Pre-saturate large
stone work surfaces consistently before applying the basecoat to support
the relief of the plaster. The qualities of the materials used to cover
building walls, roofs, and floors as envelope buildings are important
because they enclose and protect structures from the outside, deter­
mining the thermal comfort of inhabitants [1,2]. Preventing unfavorable
climatic conditions has long been a priority for people everywhere; for

* Corresponding authors at: Scientific Research Centre, Soran University, Soran, Kurdistan-Region, Iraq (C.Y. Rahimzadeh).
E-mail addresses: chiyarahimzadeh@soran.edu.iq (C.Y. Rahimzadeh), ahmed.mohammed@univsul.edu.iq (A.S. Mohammed).

https://doi.org/10.1016/j.conbuildmat.2022.128921
Received 25 May 2022; Received in revised form 8 August 2022; Accepted 17 August 2022
Available online 24 August 2022
0950-0618/© 2022 Elsevier Ltd. All rights reserved.
C.Y. Rahimzadeh et al.
example, hot summer weather and freezing winter temperatures inflict
discomfort [3]. Plaster is a fundamental element in the construction
industry. It protects the exterior and interior walls from meteorological
conditions such as acid rainwater vapor and serves an aesthetic purpose
[4]. Such plaster was applied in construction buildings for thermal
insulation purposes because they include pores inside the material,
which causes the material to be light and an excellent insulator.
Furthermore, due to the numerous voids in the lightweight material,
the resultant lightweight paste has a superior thermal insulating effec­
tiveness to standard paste. Consequently, lightweight concrete has
several advantages, including lightweight and greater thermal insu­
lation, and disadvantages, including poor mechanical properties [5–7].
Bims granule plaster is a dry mortar that has been produced. Building
lime and cement specifications (DIN EN 459 and DIN EN 197-1) are
made up of a mineral binder with 2.8 % lime and 1.2 % cement,
respectively, and a natural filler that can be up to 96 % of Bims [4]. After
mixing with water, this plaster is ready to use and forms a hydraulic
bond. One of the most commonly used additives that have been used for
improving thermal insulation properties as a lightweight aggregate and
natural filler is volcanic Pumice. The main focus was on municipal solid
waste incineration fly ash (MSWI-FA) as the primary component in
artificially manufactured aggregates containing cement and ground
granulated blast furnace slag (GGBFS) in varying percentages. This was
done after the fly ash underwent a washing pre-treatment. The manu­
factured aggregates were utilized to create lightweight concrete (LWC),
which contains both artificial aggregates and artificial aggregates
blended with a negligibly tiny amount of recycled polyethylene tere­
phthalate (PET) in the form of sand. Accordingly, the possibility of
manufacturing concrete with higher thermal and mechanical qualities
by effective PET recycling was investigated, with favorable impacts on
the thermal insulation of buildings. Based on the results, the samples
containing artificial aggregates had lower compressive strength (up to
30 %) but better thermal performance (up to 25 %) than the reference
sample made from natural aggregates. Moreover, substituting 10 % of
recycled aggregates with PET led to a more significant reduction in
resistance while improving the thermal conductivity. This type of con­
crete could improve the economic and environmental aspects by
incorporating industrial wastes—mainly fly ash—thereby lowering the
use of cement, which would lead to a reduction in CO2 emissions [8].
Volcanic Pumice deriving from acidic lavas is a highly vesicular
mineral material. It is mostly composed of amorphous silica and is
widely applied in various industries. Pumice is an igneous rock with a
cellular structure. As a result of its lightweight and insulating charac­
teristics, it has been frequently utilized in building construction [9]. The
flexural strength in pre- and post-crack, toughness, and stiffness of the
developed composites were assessed in addition to tests for unrestrained
drying shrinkage. The results obtained from those programs were
analyzed and compared to identify the optimal composite and potential
applications. The experimental analysis results confirmed the feasibility
of using this textile waste composite as a potential construction material
in non-structural concrete structures such as facade cladding, raised
floors, and pavements. The optimal composite was proven to be rein­
forced with six layers of nonwoven fabric, with a flexural strength of
15.5 MPa and a toughness of 9.7 kJ/m2 [10]. Using recycled materials
and wastes as cement reinforcement within the building sector can play
a relevant role in sustainability from environmental, economic, and
social perspectives. This study investigated the mechanical design
properties of cement pastes reinforced with short textile waste fiber
(TWF) in contents ranging from 6 to 10 percent by weight fraction
cement. These properties included flexural and compressive strengths at
7, 28, and 56 days and toughness and stiffness. The results were
compared with those obtained from Kraft Pulp pine Fiber (KPF), taken as
reference. The main conclusion is the feasibility of using this type of
fiber as potential reinforcement in construction materials with the op­
timum dosage of 8 % [11–14]. The molecular simulation of cement-
based materials is a practical approach to studying the properties and
2
Construction and Building Materials 350 (2022) 128921
interactions of the cement system at the fundamental scale. Recently,
many studies have been published regarding atomistic simulations to
investigate the cement phases to define/explain the microscopic phys­
ical and chemical properties, thereby improving the macroscopic per­
formance of hardened binders. The molecular simulation
of cementitious systems research involves researchers with multidisci­
plinary backgrounds, mainly in cement chemistry, where the hydration
reactions govern most of the chemical and physical properties at the
atomic scale, and computational materials science and engineering,
where the bottom-up approach is required. The latter approach is still in
its infancy, and a study of the prevailing knowledge is useful through an
exhaustive literature review. This state-of-the-art report provides a
comprehensive survey of studies conducted in this area and cites the
important findings [15]. The optimal dosage of polystyrene bead (EPS),
low-density polyethylene (LDPE), vermiculite (VL), and volcanic scoria
(VS) was initially determined to produce concrete blocks with low
thermal conductivity and acceptable compressive strength using low ­
cement content to reduce both the CO2 emission and the cost. Thermal
conductivity, compressive strength, density, absorption, cost analysis,
and CO2 emission were used to assess the efficiency. The results proved
that the thermal conductivity of vS EPS, LDPE, and VL blocks were
reduced by about 26.1, 19.4, 17.0, and 16.7 %, compared to the normal
block. However, the results showed that the reduction in compressive
strength was 51, 47, 39, and 37 % for vS VL, LDPE, and EPS blocks,
compared to that of the control block. Further, the vermiculite block
exhibited the highest water absorption of all blocks by up to about 14 %.
Moreover, the cost analysis results proved that the EPS and vS are the
cheapest insulated blocks compared to others. Besides, the results sup­
port the recommendation to use VS-insulated block because of its lowest
thermal conductivity, and it satisfied the requirements of compressive
strength as non-load bearing walls. It is found that the best wall (VS) can
improve the thermal resistance by about 279 % when compared to
conventional concrete blocks. This improvement could reduce the cost
of energy consumption from 349.3 to 99.4 $/m2 (about 3.5 times of
reduction) based on net present value (NPV) over 50 years. The VS-wall
could minimize the CO2 by about 3.71 times over the conventional
concrete block and about 1.35 times over the control wall. This work has
achieved the following dual benefits: converting waste polymers into
useful materials to produce cheap and sustainable constructional ma­
terial as well as saving energy and thus the environment [16–19]. Ad­
vantages of lime plaster are: Lime plaster is set to a solid mass that is
durable and relatively flexible, It is permeable and allows for moisture
diffusion and evaporation; it is less affected by water and will not dry or
dissolve like clay or gypsum plaster, Plasters made of hydrated lime are
less brittle and less prone to breakage, which does not require expansion
joints, The high pH of lime acts as a fungicide preventing mold from
growing in the lime plasters, Disadvantages of lime plaster are: Hy­
draulic lime plaster is not as hard as cement plaster When the plaster
dries, the pH drops to 8.6, Non-hydraulic lime plaster requires moisture
to set and prevents it from drying for several days.
In some countries, cement mortar is still used for external plastering;
the Bims granule-based plaster is an ideal alternative for cement plas­
ter due to its excellent thermal characteristics.
The main aim of this study is to characterize the Bims plastering
material using microstructure tests. The stress–strain behavior was
assessed using three different mathematical models at two w/b ratios up
to 28 days of curing time. The performance of the proposed models was
compared and evaluated using statistical parameters such as coefficient
of determination (R2), root mean square error (RMSE), and mean ab­
solute error (MAE).
The purpose of this study is to locate and characterize a lime-based
plaster that could potentially replace cement-based plaster, typically
used for thermal insulation. Weight loss at high temperatures can be
used to evaluate how well the LP performs and to determine the
chemical composition of the LP. Microstructure tests, including SEM
images and heat flow, identified the structure and morphology of the
C.Y. Rahimzadeh et al. Construction and Building Materials 350 (2022) 128921

Fig. 1. The flowchart of the current study.

hydrated LP and powder states. Three efficient models are used to statistical parameters such as coefficient of determination (R2), root
forecast the compression stress–strain behavior. mean square error (RMSE), and mean absolute error (MAE).

2. Methodology
2.1. Materials

The procedure followed in this study can be summarized in steps as

The plaster material utilized in this research is called “Bims” wall
follows (Fig. 1).
plastering material (LP). This section utilized six sieves ranging from 63
Step 1: The microstructure tests were performed to evaluate the
μm to 2 mm (Fig. 2). The LP particle size used in the experiment varied
chemical composition, such as thermal behavior and morphology of LP.
up to 4 mm. Approximately 30 % of the constituent particles were
Step 2: Prepared specimens using two different w/b 0.75 and 0.90 at
smaller than 63 μm in diameter, and around 20 % were between 2 mm
curing times of 3, 7, and 28 days.
and 1 mm. The LP additionally contains 1 % by weight of carbon fibers
Step 3: The initial setting time for the LP was performed.
with a diameter of 40 μm and a maximum length of 2 cm. In this study,
Step 4: Evaluate the effect of curing time on the compressive
tap water with a pH of 7.2 was used.
stress–strain behavior.
Step 5: The scanning electron microscopy (SEM) test was also con­
ducted for fractured specimens after failure. 2.2. Microstructure tests
Step 6: Three different models were utilized to predict the stress–­
strain behavior of the material. In the categories of construction materials, binders were more often
Step 7: The performance of the models was evaluated using different studied to be evaluated by XRD, XRF, and FTIR [20]. However, the SEM,
EDX, and DSC/TGA were also conducted to investigate morphological,

3
C.Y. Rahimzadeh et al.
Fig. 2. Different grain size of LP a) LP > 2 mm, b) 2 mm ≥ LP > 1 mm, c) 1 mm ≥ LP > 500 μm, d) 500 μm ≥ LP > 250 μm, e) 250 μm ≥ LP > 63 μm, f) 63 μm ≥ LP at
room temperature.
elemental mapping, and thermal properties.
2.2.1. Chemical analysis (XRF and EDX)
X-ray fluorescence (XRF) is a non-destructive test that can identify
almost any element’s X-ray emission depending on the X-ray wavelength
and intensity. At this point, a powder sample was chosen, and an XRF
test was performed. Then 100 g of LP was sieved into six different sizes
to determine the dispersion ratio of its chemical elements to grain size
(Fig. 2).
Energy-dispersive X-ray analysis (EDX) spectroscopy is also a
powerful technique that enables the user to analyze the elemental
composition of the desired sample. The major operating principle that
allows EDX to function is the capacity of high-energy electromagnetic
radiation (X-rays) to eject ’core’ electrons (electrons that are not in the
outermost shell) from an atom. The interaction of electrons with the
specimen produces X-rays (with energies characteristic of atomic num­
ber), which are detected as a function of wavelength.
2.2.2. X-ray diffraction (XRD)
XRD usually offers data on the crystalline structure, the structure’s
essence, lattice parameters, grain size, and grain density of the crystal­
line. The utilized XRD machine in this study was PW3373/00. The de­
vice specification is a Cu anode with a wavelength of 0.154 nm, max:
2.2 kW, 60 kV.
2.2.3. Thermal analysis (DSC/TGA)
Thermogravimetric analysis (TGA) was used to investigate the
thermal decomposition behavior with a simultaneous thermal analyzer
of the LP material composites. The 2.3010 mg of the samples were
heated under an argon atmosphere at a rate of 10 ◦ C min-1 from 25 to
1000 ◦ C for 5 min to eliminate any thermal processing. After that,
samples were cooled to room temperature at 10 ◦ C min− 1 under an
4
Construction and Building Materials 350 (2022) 128921
Argon atmosphere.
2.2.4. Fourier transform infrared spectroscopy (FTIR)
FTIR spectroscopy can identify the chemical bonds and structures by
utilizing infrared light. FTIR characterization was carried out using a
Thermo Nicolet 8700 FTIR spectrometer outfitted with a Smart Orbit
accessory and a horizontal attenuated total reflectance (ATR) accessory
(single reflection) outfitted with a diamond crystal in the wavelength
range of 4000 cm− 1 (2.5 µm) to 400 cm− 1 (25 µm) in an atmosphere with
decreased CO2 and H2O concentrations.
2.2.5. Scanning electron microscopy (SEM)
SEM analysis was used to describe the surface topography and
composition of the sample of the materials at micro and nano size. The
surface of a sample was coated with 200 A◦ of gold to enhance the SEM
image qualities. Then the sample was bombarded with a finely focused
(100–5 μm diameter) electron beam with an acceleration voltage of 20
kV under vacuum.
2.3. The initial setting followed ASTM C403
The initial setting time of cement is defined as the time elapsed be­
tween the moments when water is added to the cement and when the
cement paste starts losing its plasticity. The initial setting time of the
lime-based plaster is measured between adding water to the binder and
the point at which the paste appears to lose its plasticity. The room
temperature and water were maintained at a constant temperature of 25
± 2 ◦ C. The humidity level in the lab was 65 ± 5 %. At least three
samples were tested for each condition, and the mean values were taken
in the analysis.
C.Y. Rahimzadeh et al.
Fig. 3. Chemical composition of LP powder, a) XRF test, and b) EDX analysis.
2.4. Compression test
The specimens were prepared in a cylinder shape with 68 mm
diameter and 136 mm height. All of the specimens were air-cured and
kept at lab temperature. The different trials were conducted to deter­
mine the suitable w/b ratio; for this case, two different w/b (0.75 and
0.90) were performed.
The loading machine was a universal servo-hydraulic testing ma­
chine with a capacity of 2000kN; the uniaxial compression test was
performed following ASTM standards. The stress rate of the compression
machine was 0.3 MPa/s. The ends of the samples were smoothed using a
grinder machine. The test was performed using a stress rate of 0.02
MPa/s. A digital dial gauge with an accuracy of 0.01 mm was used to
measure the displacement of the device. The axial load and deformation
of the LP specimens were precisely recorded. Three samples were tested
in each case to record more accurate and realistic results.
2.5. Modeling
2.5.1. β model
Ezeldin [21] proposed an analytical equation Eq. (1) to generate the
stress–strain curve for the normal strength of steel fiber reinforced
concrete based on Eq. (1) for uniaxial compression of plain concrete.
This equation involves a material parameter β: the slope of the inflection
point at the descending branch of the shear stress relationship. This
proposed model is simpler and agrees more with the experimental data
5
Construction and Building Materials 350 (2022) 128921
than the stress–strain relationship models proposed by other researchers
[21,22]. In this work, the model of Equation (1) and the consequences of
strain and stress at the failure point were examined.
⎡ ⎤
( )
⎢ ε ⎥
β εf
σ=⎢ ⎢
⎥
( )β ⎥*σf (1)
⎣ ε ⎦
β − 1 + εf
where σ and σf represent stress and stress at failure, ε and εf indicate
strain and strain at failure, and β represents the model parameter of the
stress–strain curve. Furthermore, as β increases, the slope of the curve
increases.
2.5.2. Vipulanandan p–q model
Vipulanandan p–q Model [23–26] presented a model for predicting
the stress–strain behavior of concrete, mortar, and paste during strain
softening. The Vipulanandan p–q model was utilized to predict the
stress–strain behavior of LP as Eq. (2).
⎡ ⎤
ε
⎢ ⎥
σ=⎢
εf
⎥*σf (2)
⎣ (p+q) ⎦
q + (1 − p − q) εεf +p(εεf ) p
where σ is the stress, ε is the strain, the p and q are model parameters,
and εf the maximum strain of the sample corresponds to the failure stress
(σf ).
Parameter q was defined as the ratio of secant modulus at peak stress
to initial tangent modulus. Parameter p was obtained by minimizing the
error in the predicated stress–strain relationship. Hence, parameters p
and q in (Eq. (2)) were determined based on the stress–strain behavior of
LP with two different water/binder ratios. The values and coefficient of
determination (R2) and RMSE are summarized in Table 3.
2.5.3. Rational model
This study selected this model as the third most successful conven­
tional model used in comparable studies. Eq. (3) is a model that has
demonstrated excellent predictive ability for the stress–strain behavior
of cement-based materials [27,28]. The rational function model is a
generalized polynomial model with the following definition:
a + bε
σ= (3)
1 + cε + d ε2
where σ represents stress, ε indicates strain, and a, b, c, and d are the
equation parameters. The parameter “a” is the intercept value of the
curve in the direction of the Y axes, and the others are the form pa­
rameters of the stress–strain curve of the LP. Furthermore, the parameter
“c” must have a negative value.
3. Results and discussion
3.1. Chemical composition (XRF and EDX)
Fig. 3 contains the results of the XRF and EDX analysis, which show
the ratio of chemical compounds in the LP and confirm the results of
each other. As shown in Fig. 3a, SiO2 with 46 % is the highest element,
and CaO with 23 % is the second-highest composites rank.
The different sizes of LP material were evaluated using XRF analysis
to determine the chemical composition of LP material at different sizes
ordered from a to f. The chemical composition results are presented in
Table 1. It is observed that in part f where the particles size is less than
63 μm and constitutes 30 % of the LP, the amount of SiO2 is less than that
of CaO, and it was also found to have a greater share of calcium oxide in
the grading less than 500 μm (d–f sections).
Additionally, it is noted that all compounds are in the metal oxide
C.Y. Rahimzadeh et al. Construction and Building Materials 350 (2022) 128921

Table 1
Chemical composition for different sizes of LP.
LP SiO2 % Al2O3 % CaO % K2O % MgO % Fe2O3 % Sulfur % P2O5 % Zr % Others %

a 48.039 8.698 21.481 3.452 1.589 0.545 0.064 0.03 0.032 16.07
b 58.657 11.817 9.043 2.569 1.845 0.533 0.079 0.04 0.023 15.394
c 52.187 10.336 8.717 2.243 2.363 0.657 0.108 0.036 0.024 23.329
d 40.522 10.598 35.702 0.92 5.303 0.207 0.776 0.055 0.02 5.897
e 47.242 9.219 31.797 1.894 3.03 0.166 0.133 0.12 0.015 6.384
f 27.117 10.033 34.284 0.424 7.838 0.051 1.775 0.183 0.003 18.292

Fig. 4. TGA analysis, a) Weight loss of the LP powder, b) Comparison between the major chemical composition of LP.

6
C.Y. Rahimzadeh et al. Construction and Building Materials 350 (2022) 128921

Fig. 5. Heat flow test for LP powder using differential scanning calorimetry (DSC).

Fig. 6. Fourier transform infrared spectroscopy (FTIR) test for LP powder.

state. One of the basic properties of metal oxides is to increase the
alkaline environment in water. In other words, as the compounds are
dissolved in water, the pH of the solution increases. The lime plaster is
composed mainly of quartz, calcium carbonate, and calcium hydroxide,
with some evidence of the presence of magnesium hydroxide and
magnesium carbonate. The presence of calcium hydroxide was detected
by an endothermic peak in the TGA curves at 510 ◦ C. If the loss in mass
determined by TG, between 410 and 600 ◦ C, were to be attributed
entirely to the decomposition of calcium hydroxide, The sample might
contain >40 % Ca(OH)2. Two reasons for doubting that amorphous Ca
(OH)2 might be present were revealed when the lime plaster samples
were prepared. (i) silica and calcium carbonate (ii) silica, calcium car­
bonate, and various magnesium compounds, including the hydroxide
and carbonate and perhaps the oxide. The plasters with low magnesium
contents do not show the endotherm at 510–570 ◦ C and certainly do not
contain much Ca(OH)2.
3.2. Thermal analysis (DSC/TGA)
Fig. 4a shows the TGA curve of the LP. The result shows a total
weight loss of 16.6 % at 1000 ◦ C for the LP that has not yet reached the
degradation temperature. As shown in Fig. 4b, the main compound that

7
C.Y. Rahimzadeh et al. Construction and Building Materials 350 (2022) 128921

Fig. 7. Scanning electron microscopy (SEM) images of LP at powder state at different sizes (a) 100 μm, (b) 50 μm, and (c) 5 μm.

ultimately affects the stability of the LP at this temperature is SiO2. decomposition of MgO at 545 ◦ C. Weight loss after 550 ◦ C could also be
However, the downward movement of weight loss began at 550 ◦ C due to the complete decomposition of CaO, which occurs at 680 ◦ C,
[30–32]. The experimental sample at this temperature had lost only according to the obvious evidence in Fig. 4b. The Ca(OH)2 in CaO is
1.96 % of its weight, which could have occurred due to the completely decomposed and destroyed. The thermal decomposition of

8
C.Y. Rahimzadeh et al. Construction and Building Materials 350 (2022) 128921

Fig. 8. Stress–Strain relationship at 3, 7 and 28 days of curing.

Fig. 9. Stress–Strain relationship at 3, 7 and 28 days of curing.

Portlandite, Ca(OH)2, has been studied in air and vacuum using X-ray
single-crystal techniques. The crystals were decomposed in situ on the
goniometer arcs in the air, while X-ray reflections were recorded
simultaneously. Due to the high nucleation rate of CaO crystallites in air,
topotaxy was not followed by the change to CaO. Due to the high
nucleation rate of CaO crystallites in air, topotaxy was not followed by
the change to CaO. Due to the high nucleation rate of CaO crystallites in
air, topotaxy was not followed by the change to CaO. Due to the high
nucleation rate of CaO crystallites in air, topotaxy was not followed by
the change to CaO. When Ca(OH)2 single crystals were decomposed
under vacuum (and subsequently exposed to X-rays), some orientation
of the CaO crystallites occurred. These results are compared with those
of previous workers using electron-diffraction techniques. Decomposi­
tion of Ca(OH)2 single crystals commences at 450 ◦ C in air and 230 ◦ C in
a vacuum of 10–6 mmHg; reaction commences at crystal edges and
surface defects, the reaction boundary moving inwards to the center of
the crystal. This observation is consistent with a homogeneous mecha­
nism of decomposition [29]. Another important point inferred from
Fig. 4a is that the test specimen has the highest thermal stability of up to
150 ◦ C, meaning good thermal resistance in the hottest climate at
ambient temperature.
Fig. 5 illustrates the DSC curves of the LP and its composites. DSC

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C.Y. Rahimzadeh et al. Construction and Building Materials 350 (2022) 128921

Table 2
Model parameters for LP at different curing times and various water-to-binder ratio.
Curing Water to binder Strain corresponding to maximum Stress at failure Modulus of Model parameters
time ratio stress εf σf Elasticity Ei β Vipulanandan Rational
p-q

[Days] [w/b] (%) (kPa) (MPa) β p q a b c d

3 0.9 1.172 290 27.79 4.37 0.85 1.58 0.01 0.12 − 1.22 0.67
7 0.9 1.319 320 27.10 4.38 0.85 1.69 0.01 0.12 − 1.07 0.54
28 0.9 1.914 350 20.46 6.38 0.17 1.17 0.01 0.07 − 0.85 0.28
3 0.75 1.064 650 67.50 2.85 1.35 1.30 − 0.01 0.56 − 0.83 0.73
7 0.75 0.780 710 99.27 3.18 1.50 1.47 − 0.01 0.76 − 1.22 1.35
28 0.75 0.389 890 264.75 2.61 1.00 0.97 − 0.03 2.55 − 1.91 5.57

Fig. 10. Stress–strain relationship using different predicted models with various curing times of (a) 3 days, (b) 7 days, and (c) 28 days.

analysis can calculate various characteristics, including glass transition
temperature, vapor temperature, melting temperature, degree of
supercooling, and crystallinity [30]. The DSC curve in Fig. 5 shows an
endothermic peak around 102 ◦ C and three exothermic peaks at 97, 124,
and 150 ◦ C, respectively. Every-one of them happened within a short
distance from each other. Since the endothermic peak’s temperature is
near the boiling point of water, it can be attributed to the desorption of
water from the precursors. The glass transition stage is responsible for
exothermic development. As shown in Fig. 5, after 150 ◦ C, it entered an
endothermic slope, probably due to silica in the sample. It shows that the
material has excellent heat capacity at high temperatures, indicating
great fire resistance. This is an important specification of the sample as a
building construction material. Lime plaster combines calcium hydrox­
ide and sand (or other inert fillers). Carbon dioxide in the atmosphere
causes the plaster to set by transforming the calcium hydroxide into
calcium carbonate (limestone). Whitewash is based on the same chem­
istry. Limestone (calcium carbonate) is heated above approximately
850 ◦ C (1600 ◦ F) to produce quicklime (calcium oxide). Water is added
to produce slaked lime (calcium hydroxide), sold as a wet putty or a
white powder. Additional water is added to form a paste before use. The
paste may be stored in airtight containers. When exposed to the atmo­
sphere, the calcium hydroxide slowly turns back into calcium carbonate
through a reaction with atmospheric carbon dioxide, causing the plaster
to increase in strength. Lime plaster was a common building material for
wall surfaces in a process known as lath and plaster, whereby a series of
wooden strips on a study work frame was covered with a semi-dry
plaster that hardened into a surface. The plaster used in most lath and
plaster construction was mainly lime plaster, with a cure time of about a
month. Small amounts of plaster were incorporated into the mix to
stabilize the lime plaster during curing. Because plaster of Paris sets
quickly, “retardants” were used to slow setting time enough to allow
workers to mix large working quantities of lime putty plaster. A modern
form of this method uses expanded metal mesh over wood or metal
structures, which allows great freedom of design as it is adaptable to
both simple and compound curves. Today this building method has been
partly replaced with drywall, composed mostly of gypsum plaster. In
both these methods, a primary advantage of the material is that it is
resistant to a fire within a room and so can assist in reducing or elimi­
nating structural damage or destruction provided the fire is promptly
extinguished. Lime plaster is used for frescoes, where pigments, diluted
in water, are applied to the still-wet plaster.

10
C.Y. Rahimzadeh et al.
Fig. 10. (continued).
3.3. Optical properties (FTIR)
The FTIR spectrum reveals its functional groups, molecule structure,
and intramolecular interactions. The FTIR spectrum of the LP is shown
in Fig. 6. The narrow peak at 459 cm− 1 in the FTIR spectrum, similar to
the pumice peak at 467 cm− 1 (Fig. 6), might have been caused by Si–O
bending strength vibrations in the SiO2 formed the structure. The pre­
vious study attributes a sorption band of about 800 and 460 cm− 1 to the
Si–O–Si bond asymmetric stretching and bending vibrations, respec­
tively [31]. Around 1070 cm− 1, a prominent peak corresponds to the
asymmetric vibration of the siloxane bond, Si–O–Si [32]. This connec­
tion serves as the silica matrix skeleton. The other significant peak was
located at around 3406 cm− 1. This peak indicated the O–H stretching
vibrations of moisture of the sample absorbed from the external
11
Construction and Building Materials 350 (2022) 128921
environment.
Additionally, the water that is absorbed from the external environ­
ment creates a deformation vibration peak of about 1620 cm− 1. The
intensities of the IR absorptions are variable. The C–C stretching vi­
brations result in varying IR intensities. Most olefin C–C stretching
bands occur between 489 and 1050 cm − 1. A very small peak in the
spectra near 1637 cm− 1 observed may be attributed to organic additives
in the plaster. The peak beyond 3423 cm− 1 is due mainly to OH
stretching and bending vibrations. This peak may be due to the contact
of water with the plasters. The characteristics peak of calcite is observed
at 1427 cm− 1 in the spectra. The vibration band around 1050–1427
cm− 1 may be assigned to the characteristic in-plane bending and sym­
metric carbonate out of plane bending vibrations of calcite and arago­
nite of the lime plaster.
C.Y. Rahimzadeh et al.
Fig. 11. Stress–strain relationship using different predicted models with various curing times of (a) 3 days, (b) 7 days, and (c) 28 days.
3.4. Scanning electron microscopy (SEM)
SEM analysis was performed to characterize the surface morphology
of the materials down to the nanoscale. The resulting images are dis­
played in Fig. 7 at three distinct magnifying sizes at 100, 50, and 5 μm
for the LP. As can be observed, most of the grains are micro and nano­
scale in size (up to 10 nm), have an irregular shape, and are equally
dispersed. The images depict a flexed bar-shaped fiber with a diameter
of almost 40 μm. Various grain shapes and sizes on the fiber surface may
indicate the interaction and compatibility of fibers with particles
12
Construction and Building Materials 350 (2022) 128921
(Fig. 7c). Fig. 7 shows an SEM photomicrograph with a magnification of
3000. EDS analysis elucidates the possibility of garnet, kyanite, quartz,
and calcite as common minerals due to the presence of Si and Ca.
However, the plaster representing the samples is shown to contain so­
dium and potassium, which might be due to the presence of salts. The
results correlate well with the chemical composition results, XRD, and
TGA analyses.
C.Y. Rahimzadeh et al. Construction and Building Materials 350 (2022) 128921

Fig. 11. (continued).

Table 3
Comparison of three different models based on RMSE, MAE, and R2 values.
Statistical evaluation parameters Models 0.75 w/b 0.90 w/b
3 Days 7 Days 28 Days 3 Days 7 Days 28Days

R2 β 0.827 0.845 0.162 0.889 0.879 0.918

RMSE(kPa) 5869.3 6593.7 8769.0 854.39 1023.79 890.52
MAE (kPa) 62.880 65.931 76.247 25.494 27.043 23.213

R2 Rational 0.983 0.986 0.989 0.998 0.996 0.998

RMSE (kPa) 564.85 590.53 711.53 12.212 30.65 22.079
MAE (kPa) 19.358 15.849 23.350 3.068 4.653 3.657

R2 Vipulanandan p-q 0.990 0.991 0.989 0.997 0.994 0.997

RMSE (kPa) 339.31 380.9 644.61 24.105 52.77 28.58
MAE(kPa) 14.864 16.681 21.865 4.270 5.668 4.491

3.5. Initial setting time
According to research, hardening, also known as carbonation, is
affected by relative humidity (RH) and temperature [33]. Because CO2
diffusion through pores is proportional to the amount of water present,
the climate might directly affect the rate of carbonation [34]. Addi­
tionally, relative humidity and temperature changes result in a variety
of reactions with lime in LP, such as the mineral transformation of
Portlandite (Ca(OH)2) to calcite (CaCO3), which has a significant effect
on the internal interactions and microstructure of lime plaster [35,36].
However, when testing plaster, the suggested laboratory curing condi­
tions of 65 (±15) % relative humidity and + 20 ± 3 ◦ C [37] are utilized,
often significantly different from the workplace environ­
ment conditions. The test results of the setting times of the plaster with
w/b ratios of 0.75 and 0.90 were 238 min and 295 min, respectively.
3.6. Compression test and stress–strain behavior
A series of cylindrical specimens were prepared under uniaxial
compression machines to investigate the influences of two different w/b
on the compression stress–strain behavior of LP. The stress–strain test
was conducted at three different curing ages. Lime plaster has been used
for building since before the use of cement. Recently, it has become more
popular because it is more environmentally friendly than cement. Lime
plaster can be made in two ways, but it does require a fair amount of
time and hard work to make it properly. As lime plaster is prepared,
careful safety attention is taken. With both recipes, mix until all lumps
are gone and run the mixture through a fine-mesh screen to remove
chunks of limestone. Store the lime plaster in a sealed container to
protect it from the air for three months before using it. With increasing
stress, several micro-fractures developed in the specimen. As additional
cracks emerged and expanded, the stress versus strain became
nonlinear. Once the stress reached its maximum value, the specimen was
immediately degraded to failure. However, the stress continued and
caused many large fractures on the specimen. The stress–strain behavior
is depicted in Figs. 8 and 9. The peak stress and strain of all curves were
the mean values of the three samples. According to Figs. 8 and 9, several
observations were made through experimental study, including the
following: (i) the elastic region of the stress–strain curve was more stable
than the plastic region (after failure [21]. (ii) The compression peak of
the specimens with w/b of 0.75 had less strain when the curing time
increased to 28 days, while the strain in the specimens with w/b of 0.90

13
C.Y. Rahimzadeh et al.
Fig. 12. Scanning electron microscopy (SEM) analysis for a failed sample at 28 days of curing time with w/b = 0.75, (a) 100 μm, (b and c) 50 μm, (d and e) 5 μm.
was increased. (iii) In general, the maximum stress of all samples of LP at
w/b of 0.75 was almost 2.6 times higher than the maximum stress of LP
at w/b of 0.90. The maximum compressive strength for the LP specimens
with 0.75 and 0.90 water-to-binder ratio at 28 days of curing time was
0.9 and 0.35 MPa, respectively (Table 2). Three different models have
been applied to predict the value of compressive stress vs strain. The
models have been proposed separately for six conditions, such as 3, 7,
14
Construction and Building Materials 350 (2022) 128921
and 28 days of curing for each w/b ratio of 0.75 and 0.90. The obtained
parameters for each model are listed in Table 2. As shown in Figs. 10 and
11, the β and Vipulanandan p-q models were able to detect the peak of
stress well. By comparing RMSE, MAE, and R2 in Table 3, the β model
has less prediction than the other two models. In terms of statistics, The
Vipulanandan p-q model detects the whole behavior of LP specimens
under stress. However, as shown in Figs. 10b, c, and 11, the rational
C.Y. Rahimzadeh et al.
Fig. 12. (continued).
model cannot accurately interpret the experimental data at failure and
after failure. According to Table 2, the modulus of elasticity of LP is 20
MPa when w/b of 0.90 and the curing time is 28 days, and 265 MPa
when w/b = 0.75 and the curing time is 28 days. The results reveal that
when the w/b ratio is dropped to 0.75 or below, the modulus of elasticity
increases significantly, 13 times more than the modulus of elasticity at a
w/b ratio of 0.90.
15
Construction and Building Materials 350 (2022) 128921
3.7. Microstructure analysis for failed samples (SEM)
Fig. 12 demonstrates scanning electron microscopy images of the
micromorphological characteristics of hydrated LP (at 28 days of curing)
after the failure of the specimen. Fig. 12a reveals an uncompacted
texture of the hydrated material with numerous large and tiny pores on a
micro-scale. The masses present at this site may be divided into two
broad groups: surface sheets with an uneven arrangement and
C.Y. Rahimzadeh et al. Construction and Building Materials 350 (2022) 128921

Fig. 12. (continued).

Fig. 13. X-ray diffraction (XRD) test for the LP after hydration.

agglomerated grains. The cleavage flakes are flexible sheets that Por­
tlandite produces during hydration [38]. The peaks of XRD analysis at
2θ = 23◦ , 29.4◦ , 35.9◦ , 39.3◦ , 43.1◦ , 47◦ , 47.5◦ , 57.5◦ , 60.6◦ , and 64.7◦
for hydrated LP sample Fig. 13 indicated that the most peaks contain
Portlandite and calcite (CaCO3) which confirm that the overall com­
posite of the material consists of these two compounds. Fig. 12b, along
with the EDX diagram for point of (I), confirms the presence of Por­
tlandite sheets was >67 % of calcium. Furthermore, in Fig. 12b, the rod
shapes represent Aragonite [39], and the white bulks represent SiO2.
Fig. 12d illustrates two distinct textures: a lighter color texture (II) that
is spongy and porous, which is known as disordered calcite [40], and a
darker color texture (III) that is solid and crystalline without any pores,
as previously mentioned this is calcium-silicate. Numerous grains (1–2
μm) are distributed like pulps on the bulk phase (III) surface. The lighter
color textures (II) are created from the combination of the pulps during
the hydration process, as shown in Fig. 12d. In addition, the temperature
and carbonation as the curing conditions severely affect completing the
reactions of calcium-silicate (C–S) bonding and calcination [12,41]. In
both textures, silica is the most abundant component according to the
EDX analysis results Fig. 12d. At the same time, the amount of calcium

16
C.Y. Rahimzadeh et al.
percentage is different for both textures; calcium was recognized as
more abundant in (II) texture.
Even though nano-pores and micro-pores in the entire texture of the
material are the reason for its excellent thermal insulation characteris­
tics [42], the presence of loose and spongy phases and, on the other
hand, the fracture lines between the calcite and Portlandite shells which
cause low compressive strength of LP.
In Fig. 12e (lower-left), there is a cumulus mass formed by high-
porosity silicon dioxide (SiO2) in thin frame structures with
completely templated two-dimensional hexagonal cylindrical pores
[43]. According to observations, the fiber strands in all failed specimens
were not broken. This shows that the fibers have a very high tensile
strength but that the binding strength between the fibers and the ma­
terial composition is quite weak. Furthermore, Fig. 12c supports that the
fiber strands had excellent tensile strength even at a larger scale of SEM
images, which indicated no fracture or cracked sign with a smooth
surface.
4. Conclusions
The lime-based plasters are extraordinarily complicated structures
comprised of multiple mortars. Lime-based plaster is frequently used in
building construction as a thermal insulator. Develop construction ma­
terials such as plasters are important because they enclose and protect
buildings from the environment, affecting the thermal comfort of oc­
cupants. The results of the provided materials for both microstructure
and mechanical properties tests can be listed as follows:
1. The XRF and EDX analysis indicated that the main composition of
the LP was SiO2 and CaO, which were mostly transformed into
calcium-silicate and CaCO3 during the hydration processes, as
shown by the XRD test results.
2. According to prior research, the chemical composition of the LP
was identical to that of Pumice. The CaO content of the LP was
22.33 % more than the CaO content of Pumice.
3. According to the TGA data, the LP had great thermal stability up
to 150 ◦ C, indicating excellent thermal resistance at ambient
temperature. The nano and micropores in SEM proved the ma­
terial’s reasonable factor for thermal stability conditions. The
graph also indicated 16.6 % weight loss at 1000 ◦ C for the LP that
had not reached degradation temperature, demonstrating the
material high heat capacity and fire resistance.
4. The FTIR data confirm that most LP is composed of SiO2, as
determined by EDX and XRF analyses. FTIR spectroscopy showed
the Si-O and Si-O-Si bonds were formed. The IR spectra showed
that our synthesized material has similar and even better features
than the reference material employed. Nano board is a new
thermal insulation material manufactured with the latest high-
tech technology, and its thermal conductivity is smaller than
still air. Under high-temperature conditions, the heat insulation
performance is 3 to 4 times better than traditional fiber insulation
materials.
5. According to sieve analysis, the LP included extremely tiny par­
ticles less than 63 µm in diameter. The SEM results revealed that
the LP also contains nanoparticles and fibers with a diameter of
roughly 10 nm and 40 μm, respectively.
6. The initial setting times of the LP plaster with w/b ratios of 0.75
and 0.90 were found to be 238 and 295 min, respectively.
7. The w/b ratio lower than 0.75 and higher than 0.90 were not
appropriate for the material.
8. According to mechanical tests, w/b = 0.75 had a maximum
compressive strength of 0.9 MPa and a low strain value,
compared to w/b = 0.9, which had compressive stress of 0.35
MPa and a high strain value.
9. The Vipulanandan p-q model was more reliable than the other
models based on a statistical and engineering standpoint, with a
17
Construction and Building Materials 350 (2022) 128921
coefficient of 0.99. Furthermore, the Vipulanandan p-q model
accurately predicted the whole stress–strain behavior of LP
specimens.
10. The curing condition of LP should be at different temperatures of
25, 45, and 60 ◦ C expecting the compressive strength to increase
with increasing the temperature.
11. Curing the samples at different pH environments to evaluate the
behavior of the materials in the pH less and higher than 7.2
(water tap).
CRediT authorship contribution statement
Chiya Y. Rahimzadeh: Conceptualization, Methodology, Visuali­
zation, Investigation. Ahmed Salih Mohammed: Conceptualization,
Methodology, Validation. Azeez A. Barzinjy: Data curation, Writing –
original draft, Writing – review & editing.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Data availability
Data will be made available on request.
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