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Natural zeolite-based geopolymers as alternative building

materials
Geopolímeros basados en zeolitas naturales como una
alternativa de materiales de construcción
Néstor Ulloa 1*,** http://orcid.org/0000-0001-7819-6670, Mirian Jiménez ** http://orcid.org/0000-0002-8047-7911,
Byron Serrano ** http://orcid.org/0000-0002-2909-8035, Carlos Serrano ** http://orcid.org/0000-0002-0653-1115

*Escuela Superior Politécnica de Chimborazo, Sede Orellana, Francisco de Orellana - ECUADOR

** Escuela Superior Politécnica de Chimborazo, ESPOCH, Riobamba - ECUADOR

Fecha de Recepción: 26/08/2021

Fecha de Aceptación: 10/12/2021
PAG 05-13
Abstract

In recent years, the use of natural zeolites to synthesize geopolymer composites (pastes, mortars and concretes) has gained increasing interest among researchers
seeking to replace partially or totally the use of ordinary Portland cement. The main objective of this paper is to broaden the information available on the development
of alternative materials, for which the present research prepared samples of natural zeolite-based geopolymer mortar as a possible building material application, in
which their mechanical properties were evaluated in terms of compressive strength. Additionally, the mix design was optimized by using two alkali activators (NaOH
14M and Na2SiO3) in different proportions, river sand as fine aggregate, and curing time and temperature. All samples were characterized by quantitative X-ray
diffraction, SEM-EDS, simultaneous TGA-DSC analysis and compressive strength. The results showed that the best mix corresponds to NaOH: 14M, Na2SiO3/NaOH:
3, activator/zeolite: 0.5, sand/zeolite: 1.5, cured at 60°C, which showed a compressive strength increase (17.3 MPa) at an early age as well as in the long term.

Keywords: Geopolymer, natural zeolite, alkali activation, durability, geopolymerization, mechanical compression

Resumen

En los últimos años, el uso de zeolitas naturales para sintetizar compuestos de geopolímero (pastas, morteros y hormigones) ha despertado gran interés entre los
investigadores que buscan reemplazar la utilización del cemento Portland ordinario de forma parcial o total. El objetivo principal de este documento es ampliar la
información disponible sobre el desarrollo de materiales alternativos, para lo cual el presente trabajo de investigación preparó muestras de mortero de geopolímero
basadas en zeolitas naturales como posible aplicación de material de construcción, en las cuales se evaluó sus propiedades mecánicas a través de la resistencia a la
compresión. Adicionalmente, se optimizó el diseño de la mezcla utilizando dos activadores alcalinos (NaOH 14M y Na2SiO3) en diferentes proporciones, arena de río
como agregado fino, tiempo y temperatura de curado. Todas las muestras se caracterizaron mediante difracción cuantitativa de rayos X, SEM-EDS, análisis simultáneo
TGA-DSC y resistencia a la compresión. Los resultados obtenidos demostraron que la mejor mezcla corresponde a: NaOH: 14M, Na2SiO3/NaOH: 3, activador/zeolita:
0.5, arena/zeolita: 1.5, curado a 60°C, que mostraron un incremento de la resistencia a la compresión (17,3 MPa) tanto a temprana edad como a largo plazo.

Palabras clave: Geopolímero, zeolita natural, activación alcalina, durabilidad, geopolimerización, compresión mecánica

1. Introduction
After water, the most common building material is, by all odds, ordinary Portland cement (OPC), due to its
traditional good binding function in mortars and concrete, and its low cost. These two factors have boosted its massive
application worldwide, where the cement industry is responsible for approximately 8% of the global carbon dioxide
emissions (Karthik et al., 2017); (Müller and Harnisch, 2008); (Nikolov et al., 2017). A large number of researches
have promoted the use of supplementary cementitious materials, with the aim of reducing the cement consumption,
such as fly ash, blast furnace slags (Karthik et al., 2017), rice husk ash (Sturm et al., 2016), metakaolin (Sore et al.,
2016), natural zeolites (Auqui et al., 2017); (Baykara et al., 2017); (Cornejo et al., 2015); (Cornejo et al., 2014);
(Nikolov et al., 2017), etc. Among these materials, natural zeolites are considered a material with high pozzolanic
activity; therefore, they are used as supplementary materials in mixed cements, mortar and concrete mixtures, thereby
demonstrating an improvement of the mechanical and durability properties (Uzal et al., 2010). The advantages of
mortars and concrete incorporating zeolites are characterized by reducing the heat of hydration, and consequently
the thermal cracking, and improving the durability properties such as the penetration of chloride ions, corrosion
speed, drying shrinkage and permeability (Bakharev, 2005); (Markiv et al., 2016). However, the partial replacement
of CPO by natural zeolites as a supplementary material is not enough to cause a great impact on the reduction of the
CPO use. Therefore, this scenario calls for innovation and development of new alternative building materials.
Geopolymers are potential substitutes for cement mixtures.

1
Corresponding author:
Escuela Superior Politécnica de Chimborazo, Sede Orellana,
Francisco de Orellana - ECUADOR
E-mail: nestor.ulloa86@gmail.com

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Geopolymers can be synthesized by the polycondensation reaction of geopolymeric precursors and alkali
polysilicates (Živica et al., 2014). The geopolymerization process implies a quite fast chemical reaction under highly
alkaline conditions on Si-Al minerals, which results in a microstructure in the form of three dimensional polymeric
inorganic molecule chains and a ring structure consisting of covalent binders of Si-O-Al-O (Nikolov et al., 2017). The
chemical composition of this geopolymer material is similar to the natural zeolite materials, but it has an amorphous
rather than crystalline microstructure (Palomo et al., 1999) (Xu and Van Deventer, 2000). Due to the lack of
standards concerning the preparation and testing of geopolymers, there is a wide range of research methodologies
for the alkali activation of aluminosilicates through geopolymerization. The most common alkali activator in the
geopolymerization process is a combination of sodium hydroxide (NaOH) or potassium hydroxide (KOH) and
sodium silicate or potassium silicate (Davidovits, 1991); (Palomo et al., 1999); (Xu and Van Deventer, 2000).
(Palomo et al., 1999) concluded that the type of activator plays a significant role in the geopolymerization
process. Reactions occur rapidly when the alkali activator contains soluble silicate, either sodium or potassium silicate,
compared to only alkali hydroxides. Xu and Van Deventer (Xu and Van Deventer, 2000) confirmed that the addition
of sodium silicate solution to the sodium hydroxide solution as an alkali activator increases the reaction between the
source material and the solution. Furthermore, after studying the polymerization of sixteen natural Al-Si minerals, they
found that, generally, the NaOH solution caused a greater degree of mineral dilution than the KOH solution. Villa et
al. (Villa et al., 2010) obtained compressive strengths of approximately 30 MPa in natural zeolite-based geopolymer
samples (clinoptilolite) activated by a mixture of NaOH and Na2SiO3 in different proportions and cured at different
temperatures; they concluded that the optimal temperature lies in the range of 40-80°C. Meanwhile, (Baykara et al.,
2017) studied the effect of the NaOH concentration and the proportions of calcium hydroxide (Ca(OH)2) and
Na2SiO3 in natural zeolite-based geopolymer samples (mordenite) cured at different temperatures, thereby obtaining
geopolymers with compressive strength of approximately 10 MPa after curing for 24 hours at a temperature of 60°C.
These authors concluded that a temperature increase has a negative effect on the mechanical properties.
The present research prepared two different natural zeolite-based geopolymer mortar samples (ZGM) as a
possible building material application, whose objective was to evaluate the mechanical properties of the samples.
Likewise, the work included the study of thermal properties and the mineralogical composition using instrumental
analytical techniques, for both the raw material and the material activated by two alkali activators.

2. Methods and Materials

2.1 Raw Materials
The zeolite was delivered with a particle size of ~250 μm, and underwent an initial drying treatment in a
furnace at 100°C for 24 hours. Following this process, its particle size was reduced in a ball mill until passing a 325-
mesh sieve (Nº ). The resulting zeolite powder was used with no further treatment.
The river sand as a sole aggregate for the ZGM synthesis was collected and dried in a period of time, and
passed through a 2 mm sieve (Nº 10) and retained in a sieve of 0.475 mm (Nº 40), which meets and complies with
the standard ASTM D 2487 (ASTM D2487, 2011). The activators used for preparing the geopolymer mortar were
selected according to the scientific literature reporting high compressive strength (Auqui et al., 2017); (Baykara et al.,
2017); (Villa et al., 2010); (Lynch et al., 2018); (Ulloa et al., 2018a). NaOH in pallets (Merck-Millipore) and Na2SIO3
were used.

2.2 Geopolymer Mortar Preparation

For the ZGM preparation, the previously homogenized mix (sand + zeolite) was activated with a solution of
NaOH at 14M and Na2SIO3. These solutions were used in proportions of Na2SiO3/NaOH: 2.5 and 3. The ZGM
samples were prepared in two different liquid-to-solid ratios (activator/zeolite: 0.4 and 0.5), with a constant sand-to-
zeolite ratio of 3:2. A mechanical HOBART N-50 mixer was used to mix the ZGM, according to the standard for
cement paste and mortar mixtures, ASTM C305 (ASTM C305-11, 2011). The obtained ZGM paste was poured into
cubic molds of 50x50x50, as stipulated by the ASTM C109/C109M-16a standard (Standard Test Method for
Compressive Strength of Hydraulic Cement Mortars (Using 2-in. or [50mm] Cube Specimens), 2016). They were
cured in the mold for 24 hours at two different temperatures, 60 and 80°C, and covered with a plastic packing to
prevent dehydration, excessive moisture loss and the thermal stress in the structure of the geopolymer mortar (Auqui
et al., 2017) ; (Nikolov et al., 2017); (Ulloa et al., 2018b). Subsequently, the samples were removed from the molds
and put at room temperature until completing a period of 7, 14 and 28 days for the respective compressive strength
tests see (Figure 1). (Table 1) shows the mix design and the proportions of the ZGM samples.

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2.3 Instrumental Analysis Methods

2.3.1 Compressive Strength

A Universal Testing Machine, SHIMADZU brand Model UTM-600KN, was used for the mechanical
compressive strength tests. The prepared ZGM samples were previously cured at the established times, with the aim
of assessing the compression force according to ASTM C109/C109M-16a (Standard Test Method for Compressive
Strength of Hydraulic Cement Mortars (Using 2-in. or [50mm] Cube Specimens), 2016). The results obtained from
the maximum mechanical strength directly determine the optimization of the alkali activators and the optimal curing
temperature.

Figure 1. ZGM synthetized and cured for 24 h at 60 and 80°C

2.3.2 X-ray Diffraction (XRD)

The composition of the mineralogical phase of the starting materials and the activated product was made
through X-ray diffraction, using a PANalytical® X’Pert PRO diffractometer. The operating conditions were at 30 mA
and 45 kV, the diffractometer scans were recorded with Bragg-Brentano geometry transmission at an angular interval
from 5 to 80 (°2Theta), with a step size of 0.02° and 2-second scanning rate per step, a conventional X-ray tube
(Cu_Kα-radiation) and a X’Celerator multichannel detector with anti-scattering protection. Moreover, the Rietveld
method was used to quantify the mineralogical and amorphous content, following experimental techniques found in
other similar studies (Machiels et al., 2014).

Table 1. Mix design for the ZGM preparation

Mix Activator Na2SiO3/NaOH Sand Zeolite

Identification /Zeolite Ratio (g) (g)
MGZ 1 0.4 2.5 112 88
MGZ 2 0.4 3 112 88
MGZ 3 0.5 2.5 112 88
MGZ 4 0.5 3 112 88

2.3.3 Scanning Electron Microscopy-Energy Dispersive Spectroscopy (SEM-EDS)

The morphological characterization and the geopolymerization degree can be differentiated from the
microstructure of each ZGM specimen through the SEM-EDS analysis. The SEM-EDS micrographs were obtained with
a Scanning Electron Microscope equipped with a FEI brand, Model Inspect S, Energy Dispersive Spectroscopy. For
the SEM-EDS analysis, powder samples were prepared; then, they were placed on an aluminum slide mounted over
an adhesive carbon disc to improve the electron transfer and no metal coating was used on the samples. The specified
operating conditions were: high vacuum, pressure of 15 Pa, acceleration voltage of 12.5 kV, and two spot sizes of
2.5 and 3 for the images.

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2.3.4 Simultaneous Thermal Analysis (TGA-DSC)

The thermal behavior and thermal stability analysis of the initial raw material and final product of all synthetized
samples were carried out with the simultaneous thermal analyzer TA Instruments STD Q-600. Powder samples were
prepared, with an approximate amount of 8 mg per each analysis. Alumina crucibles were used for both reference
and samples. The test applied the following operating conditions: temperature interval from room temperature to
1000°C, heating rate of 20°C/min and nitrogen flow rate of 100 mL/min (Duan et al., 2016) (Villaquirán-Caicedo et
al., 2015). The Advantage TA Universal Analysis software, version 4.5A, was used for analyzing and interpreting the
obtained data.

3.Results
3.1 XRD Mineralogical Characterization of Raw Materials
The natural zeolite results see (Figure 2a) show the presence of crystalline phases, mainly quartz (~39.3 %),
clinoptilolite (~34.4 %), mordenite (~16 %), and a small amount of calcite (~1.6 %). The greatest part of the
percentage of these phases correspond to zeolite type of minerals (Meier and Olson, 2001). The halo observed in
the diffractogram between positions 20 and 40 (°2Theta) indicates the presence of amorphous content (~8.7 %),
which contains the analyzed sample of natural zeolite. Regarding the river sand see (Figure 2b), two crystalline
phases were reported, mainly albite (~45.4 %) and quartz (~7.3 %) in a smaller amount, and a high percentage of
amorphous material (~47.2 %).

Figure 2. XRD Analysis of raw materials, a) natural zeolite XRD, b) river sand XRD

3.2 Mechanical Properties

(Figure 3) shows how the alkali activator proportions, and the curing time and temperature, affect the
compressive strength of ZGM specimens. It allows observing that an increase in the proportions of Na2SiO3/NaOH
and activator/zeolite favors the compressive strength in the first 7 days, compared with the rest of the strengths of the
other samples. Furthermore, the curing temperatures of both 60°C and 80°C has a positive effect on the mechanical

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strength. At 14 days, it is possible to observe again that an increase in the proportions of Na2SiO3/NaOH and
activator/zeolite in the samples significantly increase the mechanical strength and that the temperatures of 60°C and
80°C still prevail as optimal temperatures for curing the natural zeolite-based geopolymer mortar. Finally, at 28 days,
all specimens increase their compressive strength, especially the samples prepared with the activator/zeolite ratio
from 0.5 to 17.3 MPa.
In brief, as a consequence of the mix design parameters applied in this research, the best ZGM preparation
method corresponds to these specifications: activator/zeolite: 0.5, NaOH 14 M, Na2SiO3/NaOH: 3, sand/zeolite: 1.5
and curing temperature of 60°C for 24 h.

Figure 3. Compressive strength of ZGM samples

3.3 XRD Mineralogical Analysis

This analysis was carried out for the samples presenting the highest compressive strength in relation to each
preparation effect. The results of the XRD testing of ZGM specimens, in (Figure 4), show the quantification of
crystalline phases found in the ZGM. It is reported that the analyzed samples contain small and moderate amounts of
quartz and albite. The samples were obtained after the compression test for their analysis.
A quite significant aspect is the increase of the content of the amorphous phase formation in the ZGM samples
and the complete elimination of the crystalline phases found in the natural zeolite (clinoptilolite and mordenite) and
a considerable reduction of quartz, as well as the albite crystalline phase in the case of the river sand. All these
disappearing and reduced phases transform into amorphous material, which contributes to the formation of the
geopolymer mortar and guarantees that the alkali activation was successful (Auqui et al., 2017).
According to the compression analysis, the samples showing the highest mechanical strength are those
synthesized with activator/zeolite=0.5 and Na2SiO3/NaOH=3. Therefore, these are the samples presenting the
greatest amount of amorphous material, with an approximate amorphization range between ~70% and ~80%.

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Figure 4. XRD Quantitative Mineralogy

(Figure 5) shows the superposition of the diffractograms of the XRD analysis for all samples at 28 days of age
of the ZGM, in addition to the diffractogram of the natural zeolite and the river sand. It is possible to observe that all
specimens maintain similar diffractograms regarding the ZGM. The main difference among the XRD patterns of natural
zeolite, sand river and ZGM is the complete elimination of mordenite and clinoptilolite peaks, and the reduction of
the intensity of quartz and albite peaks.

Ab

MGZ4-80C-28d
10000 MGZ4-60C-28d
Qz
MGZ3-80C-28d
MGZ3-60C-28d
MGZ2-80C-28d
MGZ2-60C-28d
MGZ1-80C-28d
MGZ1-60C-28d
Arena
7500 Zeolita
Counts (cts)

5000

2500

Cpt
MOR

0
0 10 20 30 40 50 60 70 80

2Theta

Figure 5. Superposition of XRD diffractograms of ZGM samples at 28 days of age

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3.4 SEM-EDS Morphological Analysis

The SEM analysis establishes the geopolymerization degree of the ZGM samples, through the observation of the
reacting and non-reacting zeolite and river sand particles, thereby presenting a homogenous/compact product matrix
(completely reacting zeolite particles) and a heterogeneous product matrix (non-reacting zeolite particles). This
analysis was mostly undertaken with the samples presenting greater mechanical strength, due to the large number of
specimens.
The micrographs of ZGM samples prepared with activator/zeolite proportions of 0.5, which presented the
highest compressive strength, evidence an increasing homogeneity degree in their morphological structure, with very
dense and compact products, and very little porosity (see Figure 6). The effect of the higher ratio of activators to
activator/zeolite causes a greater dilution of the raw material, whose morphological matrix shows a surface continuity
of the reaction products similar to an instant freezing viscous liquid. These samples present a fully amorphous
structure, which indicates a completely compact matrix (reacting zeolite and sand particles), thereby favoring their
improved mechanical properties. This is consistent with the experimental findings previously reported in the
mechanical compression test of these samples.

Figure 6. SEM micrograph at 12000X of ZGM samples with following proportions: activator/zeolite=0.5, Na2SiO3/NaOH=3, (optimal mix
according to mechanical strength).
a) 7 days, b) 14 days, c) 28 days of age of the mortar

3.5 Thermogravimetric Analysis and Differential Scanning Calorimetry (TGA-DSC)

(Figure 7) shows the results of the thermogravimetric analysis for different ZGM samples reaching the highest
compressive strength, which evidence that all specimens maintain similar characteristics up to 1000°C. All samples
present a total mass loss between room temperature and 1000°C. This mass loss difference is attributed to the amount
of liquid activator used in each sample, where the activator/zeolite proportion of 0.5 is the series containing the
highest concentration of alkali solution; therefore, this will be the one with the highest percentage of mass loss.
Regarding the curing time, an ascending trend in the mass loss is observed, where the highest loss occurs at 7 days of
curing, because the water in the geopolymer samples does not evaporate at an early age. While at 14 and 28 days of
curing the mass loss decreases, which confirms a loss caused by water evaporation as the resting time of ZGM samples
increases. The total mass loss of the natural zeolite is lower than in the ZGM samples, mainly due to their water
content in the analyzed sample.
The greatest mass loss recorded in all ZGM specimens is observed in the range between room temperature and
200°C. This mass loss is a consequence of the evaporation of the water absorbed in the surface and the water within
the ZGM pores (Ulloa et al., 2018b); (Villaquirán-Caicedo et al., 2015); (Zhang et al., 2009). Between 200 and
600°C there was an additional minimum mass loss attributed to the water liberation by condensation/polymerization
of the Si-OH and Al-OH groups (Duxson et al., 2007); (He et al., 2010); (Zhang et al., 2009). As the temperature
rises, all ZGM samples evidence a mass change in the range between 600 and 800°C. This is due to the decomposition
of the carbonate species or decarbonation that is typical of synthesized geopolymers with a sodium-based alkali
solution (Nikolov et al., 2017); (Villaquirán-Caicedo et al., 2015).

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Figure 7. Mass loss thermogravimetric analysis

4. Conclusions
According to the effect of the two activator/zeolite ratios used herein (activator/zeolite=0.4 and 0.5), as this
proportion ratio increases, the compressive strength of the natural zeolite-based geopolymer mortar also increases.
A higher ratio of the proportion of sodium silicate to sodium hydroxide (Na2SiO3/NaOH= 2.5 and 3) produces
greater compressive strength in the natural zeolite-based geopolymer mortar. However, an excess in the proportion
of activators will cause a negative effect, which is the carbonation in the samples.
The alkali activation in the raw materials occurred while curing at temperatures of 60 and 80°C for 24 hours,
which resulted in an increase of the amorphous content. There was also a mass loss measured by TGA-DSC. These
effects were mainly caused by the concentration of alkali activators, which ensured that the alkali activation was
successful.
This study also demonstrated that an increase of the amorphous content was correlated to the increase of the
compressive strength of the geopolymer mortar, derived from natural zeolite and river sand. This mechanical
performance was mainly affected by the content of sodium hydroxide, sodium silicate, and the curing time and
temperature.
The optimal mix design and the curing time based on the compressive strength were found for the polymer
concrete preparation based on natural zeolites: NaOH: 14M, Na2SiO3/NaOH: 3, activator/zeolite: 0.5, sand/zeolite:
1.5, curing at 60°C, which evidenced a compressive strength increase both at early age and in the long term.

5. Acknowledgements
The authors wish to thank the Metrology and Materials Testing Laboratory (LEMAT, in Spanish) of the Escuela
Superior Politécnica del Litoral, ESPOL (Guayaquil-Ecuador), where all the tests described in this research were carried
out.

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