REVISTA INGENIO
Development of Oat Husk-Derived Nano-Silica for High-Performance and
Sustainable Mortar Applications
Desarrollo de Nanosílice Derivada de Cáscara de Avena para Aplicaciones de Mortero
Sostenibles y de Alto Rendimiento
https://doi.org/10.29166/ingenio.v8i2.8165 pISSN 2588-0829
2025 Universidad Central del Ecuador eISSN 2697-3243
CC BY-NC 4.0 —Licencia Creative Commons Reconocimiento-NoComercial 4.0 Internacional ng.revista.ingenio@uce.edu.ec
, (), - , . -
is study investigates the incorporation of nano-silica synthesized from agro-industrial waste—speci-
cally oat husks—into plastering mortars. Amorphous silica is extracted through chemical treatment and
converted into nano-silica via a sol-gel process, yielding 2.79%. Characterization through EDS, SEM,
TEM, and XRD conrms nanoscale silica formation. Mortars are formulated using Atena Máster type
N cement and ne aggregates from the “Copeta” quarry, veried under NTE INEN 2 536 standards.
Nano-silica is added at dosages of 0.25%, 0.50%, 0.75%, and 1.00% by cement weight. e mixtures are
evaluated in both fresh and hardened states. Fresh-state tests assess workability and ow, while compres-
sive strength is measured at 7, 14, and 28 days. Results show that 0.25% nano-silica provides optimal
performance, achieving 12.6 MPa at 28 days. Higher dosages lead to strength reduction, indicating a
performance threshold. A cost-benet analysis highlights the economic and environmental viability of
converting agro-waste into high-performance materials. e ndings underline nano-silica’s potential to
enhance mechanical properties while promoting sustainability. is research demonstrates that contro-
lled use of nano-silica from waste sources oers an eco-friendly, ecient solution for improving plaster
mortar in the construction industry.
Recibido: 29/4/2025
Recibido tras revisión: 19/5/2025
Aceptado: 6/6/2025
Publicado: 10/7/2025
Nano-silica, oat husk, sol-gel, mortar,
mechanical properties, plastering.
Este estudio investiga la incorporación de nano-sílice sintetizada a partir de residuos agroindustriales —espe-
cícamente cáscaras de avena— en morteros para enlucido. La sílice amorfa se extrae mediante un tratamiento
químico y se convierte en nano-sílice mediante un proceso sol-gel, obteniéndose un rendimiento del 2,79 %.
La caracterización mediante EDS, SEM, TEM y DRX conrma la formación de sílice a escala nanométrica.
Los morteros se formulan utilizando cemento Atena Máster Tipo N y agregados nos prove-
nientes de la cantera “Copeta”, vericados conforme a la norma NTE INEN 2536. La nano-sí-
lice se incorpora en proporciones de 0,25 %, 0,50 %, 0,75 % y 1,00 % en peso respecto al cemento.
Las mezclas se evalúan en estado fresco y endurecido. Las pruebas en estado fresco analizan la tra-
bajabilidad y la uidez, mientras que la resistencia a la compresión se mide a los 7, 14 y 28 días.
Los resultados muestran que la adición del 0,25 % de nano-sílice proporciona el mejor desempe-
ño, alcanzando 12,6 MPa a los 28 días. Dosicaciones superiores provocan una disminución en
la resistencia, lo que indica un umbral de rendimiento. Un análisis costo-benecio resalta la viabili-
dad económica y ambiental de convertir residuos agroindustriales en materiales de alto desempeño.
Los hallazgos subrayan el potencial de la nano-sílice para mejorar las propiedades mecánicas de los mor-
teros, al tiempo que promueven la sostenibilidad. Esta investigación demuestra que el uso controlado de
nano-sílice proveniente de fuentes residuales constituye una solución ecológica y eciente para mejorar
el mortero de enlucido en la industria de la construcción.
Nano-sílice, cáscara de avena, sol-gel,
mortero, propiedades mecánicas, en-
lucido.
Mohammadfarid Alvansazyazdi | Universitat Politécnica de Valencia - Spain
Alvaro Yerandi Carlosama Carde | Universidad Central del Ecuador- Ecuador
Jorge David Rosillo Pilamunga | Universidad Central del Ecuador- Ecuador
Pablo Mauricio Bonilla Valladares | Universidad Central del Ecuador- Ecuador
Debut Alexis Patrice Martial | Universidad de las Fuerzas Armadas - Ecuador
Jorge Luis Santamaria Carrera | Universidad Central del Ecuador- Ecuador
Hugo Alexander Cadena Perugachi | Universidad Central del Ecuador- Ecuador
Andrea Estefania Logacho Morales | Universidad Central del Ecuador- Ecuador
Jhon Fabricio Tapia Vargas | Constructora COVEVIM T&T S.A. - Ecuador
128
Development of Oat Husk-Derived Nano-Silica for High-Performance and Sustainable Mortar Applications
1. I
Mortar has been a fundamental component in societal
development for decades, playing a crucial role in the
advancement of civilization. As noted by Salamanca
Rodrigo [1], he rst mortar was made from stones and
mud, later evolving to clay-based mixtures. By the 19th
century, lime and sand were commonly used. Mortar is
considered a specialized concrete mixture due to its si-
milar composition, albeit with ne aggregate.
Currently, structural mortar has high demand due
to its diverse applications, such as masonry bonding and
plastering. ere are standards that outline specications
for mortar preparation in construction; however, they do
not specify on-site tests to determine its strength [2].
e search for innovative materials in the construc-
tion sector not only depends on advances in nanomate-
rials but also on the ecient management of experimental
data and systematic analysis, as demonstrated through
the application of executive dashboards for project mo-
nitoring [3].
In recent years, construction has undergone signi-
cant changes due to the emergence of nanotechnology.
Materials have evolved into “super materials,” reducing
environmental impact while enhancing their molecular
structure to become lighter, stronger, self-adaptive, and
intelligent [4]. ese materials are modied at a scale of
1 to 100 nanometers, inuencing physical, chemical, and
biological reactions to reinforce the polymer matrix and
regulate the controlled release of additives or active agents
with antimicrobial properties [5].
e successful implementation of disruptive techno-
logies, such as the incorporation of rice husk-based na-
no-silica, largely depends on organizational agility and the
ability to rapidly adapt to emerging synthesis and charac-
terization methodologies [6].
Just as the integration of information and commu-
nication technologies (ICTs) has transformed education
methodologies, the incorporation of locally synthesized na-
no-silica into mortars represents a crucial step towards a
more sustainable and innovative construction industry [7].
Among all nanomaterials, nano-silica has garnered
signicant attention from the construction industry. is
is due to its superior pozzolanic activity, surpassing that
of silica fume due to its larger specic surface area. is
component reacts more eciently with calcium hydroxi
-
de (portlandite), which is responsible for producing C-S-H
gel, leading to enhanced early-age mechanical strength [8].
Given the high acceptance and interest shown by
construction researchers, this study aims to analyze
the characteristics that emerge when incorporating na-
no-silica into the mortar matrix. To achieve this, com-
parisons will be made with conventional mortar using
standard materials such as cement, water, and ne aggre-
gate. By the end of the study, the eciency of nano-silica
incorporation will be evaluated in terms of compressive
strength and permeability improvements.
1.1. Silica Mortars and Nanoparticles
1.1.1.. MORTARS
Denition and types of mortars
Mortar in the construction sector is dened as the com-
bination of three main materials: cement or any binder,
ne aggregate, and water. Oen, it is necessary to add an
admixture to the mix in order to improve certain pro-
perties of the mortar. Upon setting, the mixture exhibits
behavior similar to that of concrete.
e NTE INEN 2518 standard describes ve types of
mortar based on the classication presented by the ASTM
C-270 standard, with each type of mortar exhibiting its
own characteristics, as outlined below.
Type M Mortar: It is characterized by greater durabili-
ty compared to other types of mortars. It is used in struc-
tures that support heavy loads or are in contact with the
ground or water.
Type S Mortar: Its main characteristic is adhesion to
construction materials, such as in tile coatings for oors
and walls.
Type N Mortar: It has medium strength, making it very
useful as a binder for masonry blocks and wall coatings.
Type O Mortar: It has excellent workability but low
strength. It is recommended for use in non-load-bearing
walls of buildings with a maximum of two stories and coa-
tings that are not exposed to harsh weather conditions.
Importance of Mortar in Construction
Mortars have various applications in construction,
both in structural elements, such as in masonry buil-
dings where this binder serves to support loads, and in
non-structural elements. e most common use in our
context is for non-structural elements, such as adhesives
or coatings [9].
Mortar contributes in various ways to the preserva-
tion of a structure, such as in the use of mortars for wa-
terproong, thereby preventing damage to structural
elements that could compromise the safety of the buil-
ding. Similarly, mortar ensures the bonding of elements
like blocks used in walls that divide dierent spaces, ac-
ting as a thermal and acoustic insulator to provide com-
fort for building occupants.
e aesthetic aspect of a construction largely depends
on the nal nishes, which are achieved with mortars to
129
eliminate imperfections or provide a specic style both
inside and outside the building.
Improving mortar can aid in the evaluation of the
seismic behavior of special moment frames using nonli-
near incremental dynamic analysis [10].
Composition and Properties of Conventional Mortar
Mortar, like any construction material, possesses che-
mical, physical, and mechanical properties that vary ac-
cording to the specic needs of the construction project.
ese properties are considered from the design of the
mix to its preparation process.
Composition mortar
To prepare mortar, a binder, ne aggregate, and water are
required. In some cases, special additives or aggregates may be
used to enhance certain properties.
Properties of Mortar in the Fresh State
In their plastic state, mortars display a range of key pro-
perties that are crucial for assessing their behavior and
eectiveness during fabrication and application in cons-
truction. Among these properties, workability and con-
sistency are essential to ensure ease of handling and uni-
form application, thereby guaranteeing the quality of the
construction work. [11]
Flow
is property is measured in the laboratory. e proce-
dure involves placing the mortar in the form of a trunca-
ted cone on a vibrating table, then measuring the percen-
tage increase in diameter aer allowing the mortar to fall
25 times within 15 seconds from a height of 12.7 mm. [9]
Masonry units absorb a certain percentage of water,
so it is recommended to maintain a workability range be-
tween 130% and 150% to counteract this absorption. [12]
Water Retention
e water retention capacity of mortar is essential to en-
sure that workers have sucient time to adjust masonry
units before the mortar hardens. [13]
Water retention capacity can be increased through va-
rious techniques, such as increasing the binder content,
adding ne sand, or using water-retaining materials. [2]
Workability
is property is crucial in the mortar application pro-
cess, as good workability facilitates the worker’s task and
ensures proper positioning of the masonry, while also
preventing potential voids at the joints. Additionally, in
vertical plastering, the mortar provides good adhesion
and uniform distribution for a better nish. [2]
Hardening
e hardening of mortar is directly related to workabi-
lity. As the mortar loses water, its workability decreases,
which could be detrimental. is hardening rate can be
modied through the use of additives or techniques such
as adjusting the temperature during the setting process.
1.1.2. Properties of Mortar in the Hardened State
Compressive Strength
One of the fundamental properties is compressive stren-
gth, which is inuenced by three main factors. e rst
factor is the cement-to-sand ratio, where having a higher
amount of cement relative to sand will exponentially
increase the strength. e second factor indicates that
mortars with a high neness modulus exhibit greater
strength. Lastly, it has been established that plastic mix-
tures perform better under compression than uid mix-
tures. [14]
Absorption
e ability of mortars to absorb and retain liquids is a key
factor in their strength and durability. High absorption
can increase vulnerability to water inltration, which
could deteriorate structures and promote the appearance
of cracks, corrosion of steel reinforcement. [15]
Permeability
Permeability in mortars refers to their ability to allow the
passage of liquids or gases. A highly permeable mortar
facilitates the inltration of water and other substances,
which can lead to moisture, structural corrosion, and the
deterioration of building materials. Various factors in-
uence this characteristic, such as poor mixing of com-
ponents, application errors, or the use of inadequate or
deteriorated materials. e presence of permeable mor-
tars increases the risk of damage in areas where they have
been used. [16]
1.2. NANOTECHNOLOGY AND NANOMATERIALS.
Nanotechnology emerged in the latter decades of the
20th century, driven by the development of new ena-
bling technologies for imaging, manipulating, and simu-
lating matter at the atomic scale [17]. is eld involves
controlling matter at the nanoscale and exploiting novel
phenomena and properties, oen by combining nano-
technology with other study areas like supramolecular
chemistry [18]. By reducing material dimensions to the
Alvansazyazdi M. et. al.
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Development of Oat Husk-Derived Nano-Silica for High-Performance and Sustainable Mortar Applications
nanometer scale, particularly below 100 nanometers,
quantum eects become prominent, signicantly alte-
ring their physical, chemical, and electronic properties
[19]. e application of nanotechnology can modify
certain properties of concrete [20]. Nanomaterials are
unique as they provide a high surface-to-volume ratio,
representing the engineering of useful and functional
objects at the molecular or atomic scale [21]. Nanoma-
terials are classied into four main categories. Among
these, 0-D materials, such as Au and Ag nanoparticles
and fullerenes, exhibit all their dimensions at the nanos-
cale. Meanwhile, 1-D and 2-D materials, such as carbon
nanotubes and graphene, respectively, have one or two
dimensions smaller than 100 nm. ese latter materials
are widely used in industries such as pharmaceuticals
and electrical adhesives [22].
1.3. SILICA NANOPARTICLES
Background
Silica nanoparticles have gained widespread acceptance
and recognition worldwide due to their diverse physico-
chemical properties. Based on particle size, mesoporous
silica, ranging from 2 to 50 nm, exhibits enhanced ad-
sorption/absorption behavior for hydrocarbons and can
adsorb large molecules such as proteins [23]. In contrast,
nanoporous silica particles, which are smaller than 2 nm,
have the ability to absorb gas molecules [24]. Additiona-
lly, this material emerges as an alternative to microsilica,
which is produced through the reaction of silicon at high
temperatures [25]. e incorporation of nano-silica en-
hances performance and durability, contributing to the
reuse of alternative materials and by-products from in-
dustrial processes, thereby generating a direct environ-
mental benet [26]. It is important to note that when
using this nano-addition, cement demand decreases,
while water demand in the mix increases due to its high
specic surface area [6].
e use of agro-industrial waste, such as oat husks, for
the synthesis of nano-silica oers a sustainable alternati-
ve that reduces environmental impact and promotes cir-
cular economy practices in the construction sector [27].
e various investigations take into account dierent
sustainability problems in materials used in construction
which can be improved, having several materials from
which to choose, taking into account that the most im-
portant thing is to preserve the environment in order to
preserve our planet [28].
Characteristics
Silica nanoparticles are spherical and exhibit pozzolanic
activity. In mortars, they enhance dispersion and worka-
bility while also lling voids within the mixture.
eir incorporation increases concrete strength due
to the production of C-S-H with improved properties, as
this compound results from the reaction with portlandi-
te. Additionally, they enhance workability, as their high
specic surface area demands a greater amount of wa-
ter. Furthermore, their structure is more compact, as the
pores are lled by the small particles, thereby preventing
chemical attacks and material corrosion [29].
Methods of obtaining Silica
One of the rst methods for obtaining nano-silica was
proposed by Beck in 1992, known as the sol-gel process.
is method primarily involves forming a colloidal sus-
pension, which subsequently undergoes gelation. Du-
ring this process, hydrolysis and condensation of salts
occur with the addition of catalysts, while acids or bases
are introduced at dierent stages.
e gas-phase method involves reducing quartz in a
furnace at temperatures ranging from 1500 to 2000°C.
is process produces spherical nano-silica, commonly
obtained from the metal industry. Alternatively, nano-si-
lica can be extracted from silicon tetrachloride using hy-
drogen or oxygen at high temperatures.
e precipitation method utilizes sodium silicate
or rice husk. e ashes are heated and washed to remo-
ve acids, then further washed to reach a pH of 3. Subse-
quently, bases are added, and the ashes are washed again
until a pH of 7 is achieved, resulting in the extraction of
silica [30].
e optimization of synthesis methodologies, such as
controlling the pH and sequential acid-base reux proces-
ses, is essential to maximize yield and nanoparticle qua-
lity. Similar optimization strategies have been eectively
applied in advanced material surface treatments using
NSGA-II algorithms [31].
Ilustración 1
Process for nanosilica synthesis.
131
2. Materials and Methods
is study has characterized various resources intended
for construction, based on national standards such as the
NTE INEN and international standards like ASTM. e
materials characterized include sand as ne aggregate,
cement, and nano silica.
e process and dosing used for the analysis are pre-
sented, along with an in-depth interpretation of the re-
sults obtained from the tests conducted on mortar in both
its fresh and hardened states. Among the tests performed
are owability, compressive strength at 24 hours, 3 days,
7 days, and 28 days.
e materials used for the characterization and analy-
sis of the mortar behavior in construction are shown in
Table 1 below.
Tabla 1
Materials Used
Material Source/Specication
Fine Aggregate Copeta Quarry
Cement Master Atenas
Water EPMAPS
Oat-based Nanosilica Self-synthesis
2.1. NANOSILICA SYNTHESIS.
Separation of the husk and grain.
e methodology consisted of placing the grains in a
blender, where the blades, applying mechanical force,
separated the husk from the grain. Once this was done,
a sieve and vertical movements were used to achieve the
complete separation of both elements.
Sample weighing.
e initial weight of the oat husk is recorded in order to
determine the yield of the ashes obtained aer combus-
tion, expressed as a percentage.
Sample Pyrolysis
e ground oat husks are placed in a heat-resistant con-
tainer, such as a crucible, to undergo the heating process.
A heating mesh is placed between the heat source and
the crucible. is step is crucial to ensure the safety of the
process and to guarantee an even heat distribution. To
ensure the integrity of the container and prevent possible
fractures due to direct exposure to the ame, a heating
mesh is placed between the heat source and the crucible.
is step is critical to maintain process safety and ensure
uniform heat distribution.
Ash formation
e crucible with the ashes is placed in a mue furna-
ce, where the material undergoes a calcination process
at a temperature of 1000 °C for a period of 4 hours. is
thermal treatment allows the complete conversion of the
carbonaceous residue into ashes.
Assembly of the reux equipment.
First, the universal stand is xed to the workbench, and
the clamps are placed to secure the ask and condenser.
en, a round-bottom ask with an oil bath is mounted,
securing the ask to the stand with a clamp. Next, the re-
ux condenser is connected to the neck of the ask using
an adapter or ground joint, securing the connection with
another clamp. Aerward, the water hoses are connected
to the condenser: one for the inlet (lower part) and one
for the outlet (upper part), ensuring proper water ow.
e outlet hose is directed to a drain or container. e
heating mantle is placed to facilitate the handling of rea-
gents, and nally, the oil is evenly distributed in a pot to
ensure proper heating of the ask.
Ash reux with mineral acids
e ashes are placed in a round-bottom ask, -
lling at least half of its capacity, and are heated even-
ly using a pot with oil. e water ow in the conden-
ser is turned on to prevent vapor loss during heating.
For the hydrochloric acid treatment, 200 ml of
acid are mixed with 100 g of ashes and subjected
to reux at 120 °C for 4 hours. Aerward, the ex-
cess acid is evaporated until dryness is achieved.
In the nitric acid treatment, the dry ashes are mixed with
nitric acid in the same proportion and reuxed again for
4 hours. e excess acid is then evaporated, leaving the
ashes ready for the next step in the synthesis.
Washing of ash from acid reux with distilled water.
Aer the reux treatment, the ashes are ltered under
vacuum. To completely remove the solid from the reac-
tor, portions of distilled water are added, which are also
ltered. e solid is then repeatedly washed with disti-
lled water until the pH of the washing water is between 6
and 7, ensuring the neutralization of the acidic residues.
At this point, the ashes contain a higher proportion of
silicon dioxide.
Reux with 3M concentration sodium hydroxide.
e washed ashes, rich in silicon dioxide, are mixed with
a 3M NaOH solution (200 ml per 100 g of ashes) and sub-
jected to reux for 3 hours to ensure a complete reaction.
e mixture is then cooled and ltered under vacuum,
Alvansazyazdi M. et. al.
132
Development of Oat Husk-Derived Nano-Silica for High-Performance and Sustainable Mortar Applications
separating the solids. e ltrate, which contains sodium
silicate, is collected for storage or further processing.
Precipitation and formation of the nanosilica sol-gel sys-
tem.
e sodium silicate ltrate is neutralized with sulfuric or
hydrochloric acid until a pH of 7 is reached, generating a
nano-silica gel. e gel is then dried in an oven at 100°C
until a dry solid is obtained. Subsequently, it is washed
with distilled water until the conductivity is between 17
and 40 µS/cm, removing impurities. Finally, the gel is
dried in the oven, resulting in pure nano-silica powder
ready for use.
2.2. NANOSILICA
For the use of these particles, the synthesis of nano-silica
from oat husk was carried out using the sol-gel method.
To obtain the required amount, 4 months were spent,
resulting in 150 grams of nano-silica with good purity
according to the characterization tests performed. e
decision to conduct our own synthesis was due to the
availability of the necessary resources and to obtain real
properties along with their applications using products
found in our country, Ecuador. e oat husk was obtai-
ned from San Gabriel, the capital of the Montúfar can-
ton, in the Carchi province.
Validation of silica nanoparticles through laboratory tests.
To verify that the purity, quality, and properties of the na-
no-silica are adequate, Energy Dispersive Spectroscopy
(EDS), Scanning Electron Microscopy (SEM), Transmis-
sion Electron Microscopy (TEM), and X-Ray Diraction
(XRD) tests were conducted. ese tests will allow us
to understand the internal structure, composition, and
both physical and chemical properties.
Energy Dispersive Spectroscopy (EDS) Assay
is test allows us to perform a microanalysis and quan-
tication of the elements present in the sample, enabling
the mapping of dierent regions represented by dierent
color scales.
Ilustración 2:
Identication and quantication of chemical elements.
It works by measuring the energy and intensity of the
X-rays when the sample is exposed to the electrons from
an electron microscope, which interact with the atoms
of the sample. e X-rays emitted by the microscope are
specic to each element, allowing the images to be recog-
nized by colors [32].
Barrido Microscopy (SEM)
is test allows us to analyze the crystalline structures pre-
sent in the samples, as well as the topography on the surface,
how they interact electrically, and their chemical composition
approximately 1 μm from the top of the sample, reaching an
analytical magnication of 1,000,000 times, enabling nanome-
tric visualization [33].
Ilustración 3:
Morphology and surface topography of silica nanoparticles.
Transmission Electron Microscopy (TEM).
e analysis of TEM images of nano-silica particles
allows us to gain a deep understanding of the morpholo-
gy and structure of the nanoparticles.
e transmission electron microscope operates on the
same principle as the optical microscope, except that
it uses an electron beam to focus on the specimen and
produce the image. It has a wavelength of approximately
0.005 nm, which is equivalent to 100,000 times shorter
than the wavelength produced by light [34].
133
Ilustración 4
Morphology and structure of silica nanoparticles.
X-Ray Diraction
e principle of this method is to irradiate a sample
with a monochromatic X-ray beam so that the electrons
around the atoms vibrate under the action of the X-rays,
periodically altering the electric eld, causing each elec-
tron to act as a secondary wave source that emits electro-
magnetic waves [35].
Ilustración 5
Spectrogram resulting from X-ray diraction.
2.3. DESIGN METHODOLOGY.
Material Characterization
Initially, the characterization of the materials used in the
production of mortar cubes is carried out to establish the
mix proportions.
Granulometry
e suitability of the ne aggregate size for the mortar is
evaluated following the procedure outlined in NTE INEN
696, determining the maximum aggregate size and the
neness modulus. Sieving is performed using the sieves
specied by the standard, and the data on the mesh ope-
nings of each sieve are plotted alongside the percentage
of material passing through each one, comparing them
with the limits set by NTE INEN 2536. ree samples of
sand are prepared, and granulometric tests are conduc-
ted to verify the consistency of the obtained results.
Gráca 1
Granulometric Distribution
Material Finer than Sieve No. 200
A washing procedure is performed through Sieve No.
200 (75 µm) using a selected sample of ne aggregate,
and the loss of material is determined as a percentage
relative to the initial sample, following the procedure
outlined in NTE INEN 697.
Tabla 2
Percentage of Finer Material
Colorimetry
e content of organic impurities in the ne aggregate is
determined by immersing a sand sample in sodium hy-
droxide for one day. Aer this period, the color of the
resulting liquid is compared with a standardized color
palette, following the procedure outlined in NTE INEN
855. is test helps assess the presence of organic mate-
rials that could negatively aect the setting and bonding
properties of the mortar.
Fotografía 1:
Color Comparison for the Colorimetry Test
Alvansazyazdi M. et. al.
134
Development of Oat Husk-Derived Nano-Silica for High-Performance and Sustainable Mortar Applications
Crumbly Particles
NTE INEN 698 denes the method for determining the
percentage of crumbly particles or clay lumps in the ne
aggregate. To perform this test, the sample is immersed
in distilled water for 24 hours, aer which each particle
is manually tested by attempting to break it apart with
the ngers. e percentage of crumbly particles is then
calculated by weighing the particles that break apart and
comparing this mass to the total initial mass of the sam-
ple. is test helps assess the quality of the ne aggregate,
as the presence of crumbly particles can negatively aect
the strength and durability of the mortar.
Tabla 3
Presence of Crumbly Particles
Lightweight Particles
e percentage of lightweight particles is determined by
immersing a sample of aggregate in a high-density li-
quid, allowing the lighter particles to remain suspended.
e mass of these suspended particles is then measured
according to the procedure outlined in NTE INEN 699.
is test helps identify any lightweight materials within
the aggregate, which can aect the strength and perfor-
mance of the mortar.
Tabla 4
Presence of Lightweight Particles.
Sulfate Degradation
Following the procedure outlined in NTE INEN 863, the
specied aggregate samples are subjected to a repetitive
process of exposure and drying in a sulfate solution. Af-
ter completing the test, each sample is weighed to deter-
mine the eect caused by the sulfate exposure. is test
helps assess the aggregate’s durability and resistance to
sulfate-induced degradation, which can negatively aect
the performance of the mortar.
Tabla 5
Percentage of Loss Due to Sulfate Degradation
Specic Weight and Absorption Capacity
e specic weight and absorption capacity are determi-
ned following the procedure established in NTE INEN
856. is involves bringing the aggregate sample to the
Saturation with Surface Dry (SSD) state and measuring
its mass. en, the volume of the sample is determined,
and it is dried to measure its mass again. Finally, the re-
quired values are calculated using the formulas specied
in the standard.
Loose and Compacted Density
Following the procedure outlined in NTE INEN 858, the
samples are placed in a standardized container, both in
loose and compacted states. e mass and volume of the
ne aggregate sample are then determined.
Cement Density
According to NTE INEN 156, a Le Chatelier ask, diesel,
and a cement sample are used. By measuring the mass
and volume of the cement, its density can be determined.
e test is repeated three times to validate the results,
which are presented in the following table.
Mix Design
A mortar mix is prepared to produce 9 cubes for the
compressive strength test, following the material dosage
established in NTE INEN 488. For the mix, type N ce-
ment from Atenas is used, for which no exact quantity
is specied. An initial water/cement ratio of 0.52 is used
and adjusted until the ow required by the NTE INEN
488 standard is achieved.
Material Mixing
e procedure for preparing the mortar mix according
to the NTE INEN 155 standard includes: drying the
sand for 24 hours, sieving the cement to remove clumps,
and controlling the water temperature. 740 g of cement
and 2035 g of sand are weighed, and the water volume
is measured based on the water/cement ratio. e mi-
xing process consists of several stages: rst, adding water
and cement at low speed, then incorporating the sand,
switching to medium speed to mix, homogenizing the
135
Development of Oat Husk-Derived Nano-Silica for High-Performance and Sustainable Mortar Applications
mixture, and nally mixing again at medium speed to
achieve a uniform consistency.
Determination of the Mix Flow
According to NTE INEN 488, the ow of the mortar mix
must be 110±5, measured in accordance with NTE INEN
2502. e procedure includes cleaning and preparing the
ow table, lling and compacting the mold with mortar
in two stages, smoothing the surface, and allowing it to
rest for 1 minute. en, the mold is removed, the table is
dropped 25 times in 15 seconds, and the resulting dia-
meter is measured at four points. Finally, the measure-
ments are summed to calculate the total ow of the mix.
e mortar produced with Type N cement demons-
trates adequate workability. However, when nanomate-
rials are incorporated as a partial cement replacement, a
reduction in workability is observed, leading to decien-
cies in its fresh-state properties. [36]
Specimen Preparation
e procedure for preparing mortar cubes, according to NTE
INEN 488, includes cleaning the molds, applying release agent,
and mixing the remaining mortar at medium speed for 15
seconds. en, the molds are lled, compacted in two stages
with uniform strikes, the surface is smoothed with a trowel,
the molds are labeled, and they are transferred to the curing
chamber under controlled conditions.
Addition of Nanosilica to the Mortar Mix
e inuence of nanosilica on the compressive strength
of the mortar will be evaluated at 1, 7, and 28 days, in-
corporating 0.25%, 0.50%, 0.75%, and 1.0% into dierent
mixes. For this, the amount of nanosilica will be calcula-
ted based on the weight of the cement, partially replacing
it. e dispersion will be prepared by mixing the nano-
silica with the water before incorporating all the mortar
components. Tests will be repeated for each dosage, and
the results will be compared to determine the optimal
proportion.
As this is a specialized concrete incorporating mate-
rials such as nano-silica, a specic mixing methodology
is required to ensure proper adhesion of the nano-silica
nanoparticles within the mixture. It is recommended to
reserve a minimum amount of water to eectively dissol-
ve the nano-silica, ensuring a homogeneous blend. [37]
Curing and Compressive Strength
e curing conditions for fresh mortar typically invol-
ve maintaining a constant temperature of approximately
23°C and a relative humidity of 50% during the initial
setting phase. For hardened mortar, the samples are kept
at a temperature of 23 ± 2°C and a relative humidity of at
least 50% for periods of 4, 7, 14, and 28 days. [38]
e compressive strength test of mortar cubes accor-
ding to NTE INEN 488 includes demolding the speci-
mens without damaging them and placing them under
controlled humidity and temperature conditions. Before
the test, the dimensions of the cubes are measured and
recorded in the compression machine. e specimen is
placed in the machine, correctly centered, and the load is
applied, recording the maximum force and stress in MPa
at the moment of failure. e variation in permissible
ages according to the standard is also considered.
When incorporated into the matrix of cement-based
materials such as concrete, nanosilica has been demons-
trated to signicantly enhance performance. is study
reveals that the addition of nanosilica can increase the
strength and durability of concrete by up to four times.
Both microsilica and nanosilica exhibit high pozzolanic
activity, enabling them to regulate undesirable crystalli-
zation within the concrete matrix. [39]
Absorption Capacity
e absorption test in mortars determines the amount
of water the material can absorb within a specied time,
indicating its porosity. e specimens are cured for 28
days and then completely dried in an oven before re-
cording their initial weight (W₁). Subsequently, they are
submerged in water at room temperature for 24 hours,
ensuring the absence of trapped air bubbles. Aerward,
the specimens are removed and weighed again to obtain
the nal weight (W₂). he absorption is calculated using
the equation: Absorption (%) = ((W₂ - W₁) / W₁) × 100,
where W₁ is the dry weight and W₂ is the weight aer
immersion.
Permeability
To determine the permeability of the mortar, the contact angle
test, also known as the drop test, will be used. is test allows
us to measure the ability of a liquid to wet a solid surface [40].
It involves placing a drop on the surface and measuring
the angle formed between the tangent of the drop and
the surface of the material at the contact point. e ma-
terials and procedure are as follows.
3. Results and Discussion
3.1. YIELD.
Based on the results obtained from nano-silica,
it is considered that the yield is low; however, the
presence of silica in the oat husk is a signicant ad-
vantage. e advantage lies in the fact that being an
136
Development of Oat Husk-Derived Nano-Silica for High-Performance and Sustainable Mortar Applications
abundant agro-industrial byproduct with very low
cost, it makes it an economical and sustainable al-
ternative. is allows for the reuse of these wastes to
promote the circular economy and reduce environ-
mental impact.
3.2. ENERGY DISPERSIVE SPECTROSCOPY EDS
Gráca 2:
On the le is the composition of the nanosilica and on the right
the ash residue of synthesis síntesis.
In the graph on the le, we can discuss a high relative pu-
rity, despite the presence of sodium residues, as it shows
a high content of oxygen and silicon, both in weight and
atoms, suggesting that the material is predominantly si-
lica. e graph on the right shows that the silica content
in the sample is low, indicating that the synthesis pro-
cess has not been fully ecient in producing nano-silica.
erefore, these ashes could not be treated as they would
not contain a signicant amount of silica, considering
the time it takes.
3.3. SCANNING ELECTRON MICROSCOPY SEM
Image 1
On the le is the SEM image of the nanosilica and on the right
the ash residue of the synthesis.
e le side, we can observe that the aggregates are
spherical or nearly spherical, which is characteristic of
nano-silica synthesized by methods such as sol-gel. Ad-
ditionally, the agglomeration indicates that the particles
are interacting with each other due to electrostatic or
van der Waals attraction. On the right side, the particles
appear to have very irregular and rough surfaces. is is
typical of residues that have been subjected to high tem-
peratures but have not been fully calcined. e rough-
ness may indicate the presence of pores and gaps le as
a result of burning the organic material. Some of the ob-
served structures appear to be brous or laminar. ese
could be remnants of the original biomass, such as traces
of plant bers.
3.4. TRANSMISSION ELECTRON MICROSCOPY TEM
Image 2
On the le is the TEM image of the nanosilica and on the right
the ash residue of the synthesis.
e tests show that for the nano-silica, by performing the
following analysis, we can observe that the particle size
obtained by this methodology is 8.04 nm, which is close
to the range typically considered for nano-silica parti-
cles, which usually fall between 1 and 100 nm. On the
other hand, for the ashes, the particle size obtained by
this methodology is 143.816 nm, which is outside the
range considered for nano particles.
137
Development of Oat Husk-Derived Nano-Silica for High-Performance and Sustainable Mortar Applications
3.5. XRAY DIFFRACTION XRD
Gráca 3
Nanosilica diractogram shown.
One of the most representative peaks is found at 26.6°,
indicating the presence of quartz (crystalline SiO2), as
this position is characteristic of this material. Quartz is
one of the most common forms of silicon dioxide, which
is consistent with the fact that the sample is nano-silica.
e presence of smaller peaks could be related to the pre-
sence of other silica phases or impurities in the sample.
e incorporation of nano-silica into cementitious
matrices has been shown to signicantly enhance mecha-
nical properties by reducing porosity and improving mi-
crostructural densication, aligning with recent ndings
in high-performance mortar development [41].
3.6. PERMEABILITY
Gráca 4
Contact angle of conventional mortar and with the addition of
nanosilica.
e contact angle values obtained from the conventio-
nal mortar samples and mortar with the addition of na-
no-silica at 28 days of curing are presented. ese values
are key to evaluate the wettability of the surface, which is
correlated with the permeability of the material. e an-
gle increases with the increase in the nano-silica content,
ranging from the lowest value of 15.59° for the control
mixture, indicating a high anity of water with the sur-
face, to the maximum value of 102.06° with the addition
of 1.00% nano-silica, showing a hydrophobic trend.
3.7. ABSORPTION
Gráca 5
Absorption percentage depending on the nanosilica percentage.
e graph shows the relationship between the absorp-
tion percentage and the nanosilica content (% NS). It is
observed that as the concentration of nanosilica increa-
ses, the absorption percentage progressively decreases.
e highest absorption value (12.81%) is found in the
reference sample (PATRÓN), while the lowest value
(11.74%) corresponds to the sample with 1.0% nanosi-
lica. is indicates that the incorporation of nanosilica
reduces the absorption of the material.
3.8. COMPRESSIVE STRENGTH
Gráca 6:
Compressive strength with dierent nanosilica percentages at di-
erent ages.
e graph shows the evolution of compressive strength
(in MPa) as a function of nanosilica content and curing
time (1, 7, and 28 days). e samples with 0.25% and
0.5% nanosilica show a slight improvement in strength
compared to the reference, especially at 28 days. Howe-
ver, at higher concentrations (0.75% and 1.0% NS), the
strength tends to stabilize or even slightly decrease. is
suggests that there is an optimal point in the addition
of nanosilica to improve compressive strength without
compromising the material’s structure.
138
Development of Oat Husk-Derived Nano-Silica for High-Performance and Sustainable Mortar Applications
3.9. XRAY DIFFRACTION XRD MORTAR CUBES.
Gráca 7
e diractogram is shown on the le of the conventional mortar and
on the right with the addition of 0.25% nanosilica.
In the control sample, the high peak near 30° suggests the
predominance of residual alite or belite, indicating incom-
plete hydration (less than 100%). Additionally, the small
peaks between 18° and 34° suggest typical hydration wi-
thout substantial chemical modications. On the other
hand, with the addition of nano-silica, a reduction in the
relative intensity of the portlandite peak, typically located
around 18°, 34°, and 47° in 2θ, is observed. is reduc-
tion implies that nano-silica has reacted with portlandite
to form more C-S-H gel (calcium silicate hydrate), which
results in a denser cement matrix, thereby improving
mechanical properties. e reduction of free portlandite
means there is less material available to react with CO2
or sulfates, thus enhancing the material’s durability in ag-
gressive environments. is occurs because the reaction of
nano-silica generates products that ll the capillary pores,
reducing total porosity and improving mechanical streng-
th, which in turn leads to long-term durability.
3.10. ANALYSIS OF THE COST OF PRODUCTION OF
NANOSILICA.
According to the calculation, it is observed that producing
100 grams of nano-silica costs $368.97. When compared to
the commercial prices of Aerosil 200, which is around $161.95
for 4.5 kg in the United States, the laboratory production cost
is signicantly higher than the market value. is indicates
that at an industrial level, the methods are more ecient and
cost-eective.
. C
• e synthesis of nano-silica from oat husks using the
sol-gel method proved to be a viable process, achie-
ving a yield of 2.79%, showing a signicantly higher
eciency compared to the study conducted by the
pharmaceutical laboratory of the Faculty of Chemi-
cal Sciences at the Central University of Ecuador,
which achieved a yield of 0.98% using the extraction
and gravimetry method. is dierence suggests that
the sol-gel method optimizes the recovery of silica
from agro-industrial waste, thus improving its viabi-
lity for applications in cementitious materials. Fur-
thermore, the ability to adjust synthesis parameters
to control particle morphology and size opens new
opportunities for its incorporation into high-perfor-
mance materials.
• e characterization analysis conducted through the
EDS, SEM, TEM, and XRD tests allowed the evalua-
tion of both the chemical composition and morpho-
logy of the nano-silica and oat husk ash. e EDS
spectra conrmed the high purity of the synthesized
nano-silica, with an approximate concentration of
SiO2 (90%), while the remaining content consisted
of trace impurities. In contrast, the oat husk ashes
showed approximately 1% silica. Regarding the
images obtained by SEM and TEM, it was revealed
that the synthesized nano-silica exhibited spherical
particles with an approximate size of 8-15 nm and a
homogeneous distribution. On the other hand, the
oat husk ashes presented larger aggregates with di-
mensions greater than 100 nm. is nding suggests
that controlling the synthesis process plays a crucial
role in obtaining nanoparticles with optimized pro-
perties. e X-ray test of the nano-silica revealed
the presence of amorphous phases characteristic of
SiO2, with a broad peak at 2θ = 22°, which is favo-
rable for its reactivity in cementitious applications.
is suggests that the sol-gel synthesis method ena-
bles the production of a material with high potential
reactivity in cement matrices.
• e study on the inuence of nanosilica addition in
mortars reveals that compressive strength varies de-
pending on the addition percentage and curing time,
showing better results at lower doses. At 1 and 7 days,
the mix with 0.25% nanosilica exhibited the highest
strength compared to mixes with 0.5%, 0.75%, and
1%, while higher doses did not provide consistent
improvements. At 28 days, the trend remains, with
0.25% reaching the highest strength (12.6 MPa). is
suggests that small amounts of nanosilica optimize
strength, but higher doses may not be benecial.
• is study evaluated the economic feasibility of
producing nano-silica from oat husks, with an
approximate cost of $368.97 per 100 grams of pro-
duct under laboratory conditions, using agro-in-
dustrial waste, promoting the circular economy
and environmental sustainability. By utilizing an
abundant, low-cost waste material and the ability to
customize the properties of the material according
to its specic application, its production in labora-
tories could be justied due to particular technical
requirements. Under current conditions, however,
the production is not competitive.
139
Development of Oat Husk-Derived Nano-Silica for High-Performance and Sustainable Mortar Applications
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Annexes
Table 6
Percentage of Absorption of Fine Aggregate.
Table 7
Loose and Compacted Density of Sand.
Table 8
Average Cement Density.
Table 9
Material Dosage According to NTE INEN 488.
Table 10
Results of nanosilica synthesis.
Table 11
Nanosilica Production Cost.
Realizado por:
Proyecto:
Rubro:
Unidad:
UNIDAD CANTIDAD
PRECIO
UNITARIO
COSTO
kg 5.37 0.50 2.69
L1.13 4.00 4.54
kg 1.13 3.00 3.40
L80.00 0.50 40.00
kW/h 20.50 0.10 2.05
SUBTOTAL 52.67
UNIDAD Cantidad
Jornal
(USD/hora)
COSTO
hora 20.50 3.00 61.50
hora 20.50 2.50 51.25
SUBTOTAL 112.75
UNIDAD CANTIDAD
PRECIO
UNITARIO
(USD/h)
COSTO
C=A*B
hora 20.000 1.00 20.000
hora 150.000 1.00 150.000
SUBTOTAL 170.00
COSTO
HORA
SUBTOTAL 33.54
368.97
0
368.97
UNIVERSIDAD CENTRAL DEL ECUADOR
ANÁLISIS DE PRECIOS UNITARIOS DE LAS MEZCLAS DE MORTERO
Síntesis de nanosílice de 100 gr
gr
FACULTAD DE INGENIERÍA Y CIENCIAS APLICADAS
CARRERA DE INGENIERÍA CIVIL
Carlosama A. & Rosillo J.
Síntesis de nano sílice a partir de la cáscara de avena para modificar las propiedades físicas y
mecánicas del mortero con un enfoque eco amigable.
A. MATERIAL
B. MANO DE OBRA
C. MATERIALES
DESCRIPCIÓN
Horno de calcinación
DESCRIPCIÓN
Cáscara de avena
Ácido Sulfúrico
Hidróxido de sodio
Agua destilada
Energía eléctrica
DESCRIPCIÓN
Técnico de laboratorio
Ayudante de laboratorio
Bomba de succión al vacío
D. COSTO INDIRECTO
NOTA: ESTOS PRECIOS NO
INCLUYEN EL IVA
TOTAL COSTO DIRECTO (A+B+C+D)
COSTO INDIREC TO
COSTO TOTAL DEL RUBRO: (USD)
DESCRIPCIÓN
CANTIDAD A
10%
33.542
