ISSN 2477-9105

DOI: https://doi.org/10.47 1 87 /perf.v1i 34 .362

INFLUENCIA DE LA NANOSÍLICE EXTRAÍDA DE CAPARAZONES DE CANGREJO EN LAS

Número 34 Vol.1 (2025)

PROPIEDADES FÍSICO-MECÁNICAS DE LOS MORTEROS DE CEMENTO

Fecha de recepción: 25-02-2025 · Fecha de aceptación: 16-06-2025 · Fecha de Publicación: 24-11-2025

Alvansazyazdi, Logacho, Molina, Santamaría, Cadena, Bonilla, Lascano, Bucheli, Soledispa, Crespo, Oleas, Jiménez, Espinoza, Martial, Heredia, Tapia

INFLUENCIA DE LA NANOSÍLICE EXTRAÍDA DE CAPARAZONES DE

CANGREJO EN LAS PROPIEDADES FÍSICO-MECÁNICAS DE LOS

MORTEROS DE CEMENTO

Influence of nanosilica extracted from crab shells on the physical-mechanical

properties of cement mortars

¹^{, 2, 3}Mohammadfarid Alvansazyazdi*

2 Andrea Estefanía Logacho-Morales

² Wilson Steven Molina-Freire

⁷ Edwin Iván Soledispa-Pereira

2 Jorge Oswaldo Crespo-Bravo

² Marcelo Fabian Oleas-Escalante

³ Carmita Guadalupe Jiménez-Merchán

³ Ángel Mauricio Espinoza-Cotera

⁸ Alexis Patrice Martial-Debut

² Byron Giovanoli Heredia-Ayala

⁹ Jhon Fabricio Tapia-Vargas

iD

² Jorge Luis Santamaría-Carrera

² Hugo Alexander Cadena-Perugachi

⁴ Pablo Mauricio Bonilla-Valladares

⁵ Natali Elizabeth Lascano-Robalino

^{2, 6}Jorge Alexander Bucheli-García

¹ Universitat Politécnica de Valéncia Spain, Institute of Science and Concrete Technology, Valencia, Spain.

2 Central University of Ecuador, Faculty of Engineering and Applied Sciences, Civil Engineering Department, Quito, Ecuador.

3 Laica Eloy Alfaro de Manabi University, Faculty of Engineering Industrial and Architecture, School of Civil Engineering, Manta, Ecuador.

4 Central University of Ecuador, Faculty of Chemical Sciences, Quito, Ecuador.

5 Central University of Ecuador, Faculty of Engineering and Applied Sciences, Information Systems Department, Quito, Ecuador.

6 Pontifical Catholic University of Ecuador, Department of Civil Engineering, Quito, Ecuador.

7 Terminal portuario de Manta, Manta, Ecuador.

8 University of the Armed Forces ESPE, Department of Life Sciences and Agriculture, Center for Nanoscience and Nanotechnology,

Sangolquí, Ecuador.

9 Constructora COCEVIM T&T S.A., Quito, Ecuador.

* faridalvan@uce.edu.ec

RESUMEN

Esta investigación evalúa el uso de desechos de caparazones de cangrejo para mejorar morteros, incorporando nanosílice al

0.25% en peso del cemento como alternativa sostenible. Las nanopartículas, obtenidas de residuos biológicos, se aplicaron en

cementos Tipo N y HS, formulados para mampostería y resistencia a sulfatos. La metodología incluyó síntesis de nanopartículas,

ensayos de compresión uniaxial, pruebas de permeabilidad y análisis microestructural (XRD y SEM).

Los resultados muestran que la nanosílice incrementa resistencia y durabilidad, aunque la nanoquitina y nanopartículas de cal

fueron más eficaces a largo plazo. La mezcla C+S₀.₂₅% alcanzó 31.22 MPa a 90 días, similar a su control (31.63 MPa), mientras

que M+S₀.₂₅% aumentó un 3.2% frente a su referencia. El aumento de resistencia en edades tempranas (24 h-7 d) indica que la

nanosílice acelera la hidratación y densifica la matriz, mejorando la cohesión interna.

Las pruebas de permeabilidad evidenciaron comportamiento hidrofóbico (ángulos >90°), reduciendo la absorción de agua

y favoreciendo la durabilidad. Esta estrategia optimiza el desempeño del mortero y promueve la sostenibilidad mediante la

reutilización de residuos, alineándose con la economía circular y la nanotecnología, demostrando la viabilidad de nanosílice

derivada de cangrejo en materiales de construcción ecoeficientes.

Palabras claves: Nanosílice, mortero, resistencia a la compresión, microestructura, sostenibilidad.

ABSTRACT

This study evaluates the use of crab shell waste to enhance mortar properties by incorporating nanosilica at 0.25% by

cement weight as a sustainable alternative. The nanoparticles, obtained from biological waste, were applied to Type N and

HS cements, formulated for masonry and sulfate-resistant applications. The methodology included nanoparticle synthesis,

uniaxial compression tests, permeability assessments, and microstructural analyses (XRD and SEM).

Results show that nanosilica improves compressive strength and durability, although nanochitin and calcium nanoparticles

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proved more effective in long-term performance. The C+S₀.₂₅% mixture reached 31.22 MPa at 90 days, similar to its control

(31.63 MPa), while M+S₀.₂₅% achieved a 3.2% strength increase compared to its reference. The early-age strength gain (24

h–7 d) indicates that nanosilica accelerates cement hydration and densifies the matrix, improving internal cohesion.

Permeability tests revealed hydrophobic behavior (contact angles >90°), reducing water absorption and enhancing durability.

This approach optimizes mortar performance while promoting sustainability through the reuse of waste materials. It aligns

with circular economy principles and nanotechnology applications, demonstrating the feasibility of using crab-derived

nanosilica in the development of eco-efficient construction materials.

Keywords: Nanosilica, mortar, compressive strength, microstructure, sustainability.

I. INTRODUCTION

The integration of nanoparticles in construction

materials has gained significant attention due to

their ability to enhance mechanical properties,

durability, and sustainability. Among these,

nanosilica has emerged as a key material for

improving the performance of mortars and

concretes, primarily by reducing porosity and

increasing compressive strength (1). Additionally,

nanosilica derived from crab shells represents an

innovativestrategyfordevelopingmoresustainable

construction materials, aligning circular economy

principles by repurposing industrial by-products

and minimizing environmental impact (2).

strength, with nanoparticle dispersion playing a

critical role in optimizing mortar performance and

reducing porosity (9,10).

In addition to structural improvements, the use of

nanosilica in concrete pavers has been explored

as an alternative for sustainable infrastructure

development. Research findings indicate that a 3%

nanosilica replacement results in a 12% increase

in compressive strength, while a combined micro-

and nanosilica mix achieves a 23% improvement,

demonstratingthefeasibilityofenhancingconcrete

durability while reducing cement consumption

(11).

Furthermore,

bio-composite

materials

The incorporation of nanosilica into cementitious

matrices has been shown to promote the

formation of calcium silicate hydrate (C-S-H)

compounds, which accelerates hydration reactions

and strengthens the internal microstructure of

the mortar (2,3). Additionally, nanosilica acts as

a nano-filler, improving aggregate distribution

and optimizing material cohesion, which directly

contributes to increased durability and resistance

to external agents (4,5). Research on high-

performance concrete (HPC) indicates that a 1.5%

nanosilica replacement can increase compressive

strength by 8.44% at 28 days, significantly

reinforced with nanosilica have shown promise in

sustainable construction, as silica nanoparticles

increase strength, durability, and environmental

resistance, offering innovative solutions for eco-

friendly material development (9).

In conclusion, the utilization of nanoparticles,

particularly nanosilica, presents a significant

opportunity

to

improve

the

durability,

sustainability, and mechanical efficiency of

cementitious materials. These advancements

contribute to reducing environmental impact,

optimizing material properties, and promoting

a more resilient and eco-friendly construction

industry. As research continues to evolve, the

potential of nanotechnology in construction will

further expand, providing innovative and high-

performance solutions for the built environment.

enhancing

cement

hydration

and

matrix

densification (6,7).

Moreover, functionalized hydrophobic nano-

silica has demonstrated enormous potential

in enhancing water repellency and corrosion

resistance in cementitious materials. Research

findings suggest that substituting 2% of the

cement weight with nanosilica enhances the early-

age strength of the material and mitigates chloride

ion penetration, which is crucial in reinforced

concrete applications, particularly in aggressive

environments (8). Similarly, the integration of

nano-iron and nanosilica in mortars has been

found to enhance compressive and tensile

II. MATERIALS AND METHODS

Crab Shell-Derived Nanosilica

Background

The incorporation of nanosilica into cementitious

materials has been extensively studied due to

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its ability to enhance strength and durability in

mortar. Recent research highlights that nanosilica

obtained from crab shell waste is emerging as a

sustainable and efficientalternativeforoptimizing

cementitious mixtures. The pozzolanic activity of

nanosilica enables it to act as a nano-filler, refining

the cement matrix structure, reducing porosity,

and promoting a more compact material. This

effect translates into higher compressive strength,

with studies reporting up to 40% improvement in

nanosilica-modified mortars, indicating a notable

reinforcement of mechanical properties (12).

that nanosilica-enhanced mortars and concretes

are crucial for developing high-performance

and environmentally sustainable construction

materials (16).

The integration of nanosilica, particularly when

sourced from sustainable waste materials,

presents a promising pathway for improving the

mechanical, durability, and sustainability aspects

of cement-based materials. Given the growing

need for green construction solutions, ongoing

research will continue to explore the optimal

dosages and hybrid nanomaterial applications

to further enhance the efficiency and ecological

impact of modern construction practices.

Additionally, nanosilica contributes to reducing

mortar permeability, which is essential in

enhancing resistance against aggressive agents

such as chlorides and sulfates. This property is

particularly relevant for infrastructures exposed

to marine or industrial environments (Morales

et al. (13), the use of nanoparticles in cement-

based composites contributes to reducing

pollution and environmental impact during

production processes. Experimental studies using

X-ray diffraction (XRD) and scanning electron

microscopy (SEM) have demonstrated that

nanosilica induces the formation of additional

hydration products, particularly calcium silicate

hydrate (C-S-H) gel, which is crucial for mechanical

resistance and long-term durability (14).

Synthesis

Crab Shell

Figure 1 illustrates the process of obtaining

crab flour from crab exoskeletons through four

sequential steps:

1. Crab exoskeleton: Initial raw material

consisting of crab shells.

2. Washing and drying of crab exoskeleton:

The exoskeleton is cleaned to remove

impurities and then dried to facilitate

further processing.

3. Crushing of crab exoskeleton: The dried

exoskeleton is mechanically ground using a

milling device.

4. Crab flour: The final product is a fine powder

obtained from the crushed exoskeleton,

which can be used for various applications.

Moreover, the sustainability benefits of nanosilica

are increasingly recognized in construction

materials research. The utilization of nanosilica

derived from industrial and biological waste

sources contributes to lowering CO₂ emissions

associated

with

cement

production.

This

aspect aligns with the circular economy model,

promoting eco-friendly alternatives that reduce

the demand for natural resources while improving

material performance (15).

Furthermore, nanosilica’s nanometric scale and

high specific surface area allow for superior

cement

hydration

kinetics,

accelerating

reaction rates and improving early-age strength

development. Studies have confirmed that its

interaction with calcium hydroxide (CH) reduces

the formation of voids, resulting in a denser,

more homogeneous microstructure (14).

Figure 1. Production of Crab Raw Material

Lastly, the combination of nanosilica with other

nanomaterials,suchasnano-ironandnano-titania,

has demonstrated additional improvements in

flexural strength, impact resistance, and self-

healing capabilities. These advancements suggest

Chemically Obtained

This study investigates the extraction of nanosilica

from crab shell waste, aiming to optimize

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its synthesis for application in cementitious

materials. The research prioritizes identifying an

efficient methodology that enhances mechanical

properties

and

durability

while

aligning

with sustainable construction principles.

A

comprehensive evaluation is conducted, focusing

on process feasibility, economic viability, and the

quality of the extracted material to determine

its potential for large-scale implementation.

By refining this approach, nanosilica can be

systematically integrated into cement-based

composites, contributing to enhanced mechanical

strength, reduced permeability, and a lower

environmental footprint in modern construction.

Nanosilica from crab

Figure 2. Crab Nanosilica

For this procedure, the article "Estimation of

chitin and chitin nitrogen in crab waste and

derived products" (17) served as the basis. To

accommodate specific conditions, adaptations

were made to the method described in the

article. This approach allows for the adjustment

and optimization of the analysis process to obtain

more precise and relevant results for the study.

STRATEGIES AND MATERIALS USED

This research presents a comparative technical

analysis of the physicochemical and mechanical

characteristics of mortars formulated with

nanosilica extracted from crab shell waste and

two distinct cement types. The study aims to

assess the influence of these variables on the

overall performance of the mortar, providing

insights into their potential applications in

construction materials. The selected cements,

Type N and Type HS, are known for their

Figure 2 outlines the process of obtaining

nanosilica:

1. Sample Weighing: A portion of the dried

and ground sample is weighed. The

quantity will depend on the type of sample

and the expected fiber content.

performance

under

various

environmental

conditions and resistance to aggressive agents.

The nanosilica, obtained through a controlled

synthesis process, is evaluated for its impact on

mortar durability, strength, and permeability

reduction. The research methodology involves

assessing the influence of nanosilica on mortar

performance, considering production complexity,

cost efficiency, and final material quality.

2. Acid Digestion: The sample is dissolved

in a 1N hydrochloric acid solution in a

digestion vessel at boiling temperature for

a specified time (usually 60 minutes).

3. Filtration: After acid digestion, the mixture

is filtered through a crucible filtration or

filter cloth to collect the insoluble fraction,

which should reach a neutral pH.

4. Alkaline Digestion: The collected residue is

dissolved in a 5% sodium hydroxide (NaOH)

solution at boiling temperature for a time

similar to acid digestion.

The

experimental

phase

includes

the

characterization of mortar through standardized

tests for compressive strength, permeability,

and

microstructural

analysis,

employing

5. Second Filtration: The mixture is filtered

again to collect the insoluble fraction in the

alkaline solution.

6. Washing: The residue is washed with hot

water until the filtrate is free of acids and

alkalis.

7. Drying and Weighing: The residue is

subjected to drying in an oven at a

controlled temperature, typically between

105 and 110°C, yielding a chitin residue

contaminated with SiO₂.

X-ray diffraction (XRD) and scanning electron

microscopy (SEM). This study aims to establish the

technical feasibility of utilizing crab shell waste as

a sustainable source of nanosilica in construction,

improving mortar properties while contributing

to eco-friendly construction practices. The

comparison of results will determine the optimal

cement-nanosilica combination, offering the best

performance in terms of durability, mechanical

strength, and practical implementation in

construction projects.

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Materials

enhances the durability and integrity of

structures, contributing to safer and more

sustainable construction practices.

The characterization was carried out through

laboratory tests that comply with national

INEN standards. To create mortar specimens,

all materials used were characterized, and trial

mixes were made until official mixes were defined

based on their properties. It was necessary

to detail the mixed design and manufacturing

process. The results were subsequently applied to

mortars in both their fresh and hardened states.

The experimental procedures encompassed

flowability measurements, and compressive

strength testing, along with permeability

assessments conducted. The resulting data

underwent a thorough analysis and interpretation

to ensure comprehensive evaluation.

Fine Aggregate (Sand)

The Toachi River quarry, in the province of

Santo Domingo de los Tsáchilas, is operated by

Copeto Cía. Ltda., a company specializing in the

extraction and supply of construction aggregates

(19) . The quarry provides various types of sand,

including washed sand, block sand, and natural

sand, all of which meet the highest national

quality standards (INEN, MOP) and comply with

international regulations (ASTM) (20).

Table 2 outlines the physical characteristics of

the fine aggregate, reporting a fineness modulus

of 2.44. Furthermore, Figure 3 illustrates the

particle size distribution curve, which aligns with

the requirements established by NTE INEN 2536

(21) for its application in masonry mortar.

The study focused on the characterization of

mortars composed of fine aggregate (sand),

cement, and nanosilica synthesized from crab

shell waste, as outlined in Table 1. These materials

were integral to assessing the performance and

properties of the developed mixtures.

Table 2. Characteristics of Fine Aggregate.

Characteristics

Colorimetry

Units

Results

1

Table 1. Components used

-

Materials

Specification

Origin

Fineness Modulus

Specific Gravity

Absorption Capacity

-

g/cm³

%

2.44

2.70

1.50

Fine

Aggregate

Quarry of Copeto

Toachi River

Type N Masonry

Cement

Holcim

Portland Pozzolanic

UNACEM

Type HS

Metropolitan District of

Quito Water Network

(EPMAPS)

Water

Drinkable

Crab

Nanosilica

Synthesized Material

Laboratory-Synthesized

Water

The amount and quality of water incorporated

into the mortar mixture are fundamental factors

in determining its mechanical characteristics and

long-term durability. The use of clean, impurity-

free water is vital for effective cement hydration,

which directly affects the mortar's ability to meet

the required mechanical standards. In contrast,

water of inferior quality can adversely affect

these properties and reduce the workability of

the mixture.

Figure 3. Granulometric of aggregate

Cement

Portland Pozzolanic Cement is a blended material

composed of Portland Cement and pozzolanic

additives, which are reactive compounds derived

either from natural volcanic sources or synthetic

processes (22). This cement variant exhibits

improved durability against chemical exposure,

lower heat of hydration, and enhanced water

resistance compared to standard Portland

Cement.

Therefore,

adherence

to

the

NTE

INEN

2617:2012 standard (18) is essential to ensure

that construction water meets the necessary

requirements. Compliance with this standard

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In this study, Type N and HS Portland Cement,

conforming to the specifications outlined in NTE

2380 (23), (24), were selected to evaluate their

performance in mortar formulations.

Composition of crab nanosilica through

laboratory tests

Laboratory tests were performed to verify the

composition of the nanoparticles extracted from

crab exoskeletons and assess the effectiveness

of the research. The analysis involved Energy

Dispersive Spectroscopy (EDS), Scanning Electron

“Maestro” Cement – Holcim Type N

Holcim "Maestro" Type

N

cement is an

advanced, high-performance material specifically

engineered for modern masonry applications.

Its optimized formulation improves workability

by up to 15% compared to traditional cements,

effectively reducing material loss and rebound

during application. Additionally, its superior

waterproofing capability, ranging from 65%

to 90%, makes it particularly well-suited for

structures subjected to constant moisture

exposure (24).

Microscopy

(SEM),

Transmission

Electron

Microscopy (TEM), and X-ray Diffraction (XRD).

These characterization methods are essential

for evaluating the properties and structural

composition of the crab-derived nanoparticles.

Scanning Electron Microscopy (SEM) and

Energy Dispersive Spectroscopy (EDS)

Testing

Crab Nanosilica

“Campeón” Cement - UNACEM Type HS

In Figure 4, the SEM images (a)-(b)-(c)-(d) offer a

detailed analysis of the morphology and particle

distribution within the sample, providing valuable

insights into its structural characteristics. The

combinationoflaminarandparticulatestructures,

along with rough and fractured textures, suggests

that the material has a complex nature, possibly

with different phases: fibrous or porous. The

variability in particle size and distribution may

have significant implications for the material's

physical and chemical properties, such as

reactivity, porosity, and mechanical strength.

“Campeón” HS cement is a high-sulfate-resistant

hydraulic cement certified under the NTE

INEN 2380 standard to guarantee quality and

reliability in construction. Its high fineness and

precisely controlled composition enable the

production of long-lasting concrete, particularly

in aggressive environments with elevated sulfate

concentrations in soils and water. This cement is

especially suitable for applications such as mass

concrete structures, soil stabilization, dams, and

mortars that are easy to place and provide high-

quality finishes (25).

Ultrasound

Ultrasound has proven to be an efficient method

for dispersing nanoparticles within cement-based

matrices. Research has shown that ultrasonic

treatment promotes a more uniform distribution

of nanoparticles in the mortar, resulting in a

denser and stronger microstructure. For instance,

research (26) suggests that the application of

ultrasound can promote the growth of C-S-H

phases in cement paste, thereby improving

mechanical strength and reducing porosity (27).

Nanoparticles obtained from crab shells

The nanoparticles were synthesized at the UCE

laboratories, where 1,000 grams of pure crab

meal derived from exoskeletons were processed.

Following a series of chemical treatments,

129 grams of crab-derived nanosilica were

successfully extracted.

Figure 4. Morphology and topography of crab nanosilica

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Energy dispersive spectroscopy (EDS) is an

analytical technique used to characterize the

chemical composition. It is particularly valuable

in the analysis of nanomaterials, as it enables

the detection and quantification of the elements

present within the material.

The analysis was conducted employing a

diffractometer over a 2θ scanning range from

0 to 90°, at a scan rate of 0.02 degrees per

second. Distinct diffraction peaks were observed

around 2θ = 22° and 27°, characterized by their

sharpness and high intensity, clearly indicating

a high crystallinity level and confirming the

presence of silica in its nanostructured form.

As illustrated in Figure 5, the analysis identified

and confirmed the presence of key elements:

The

XRD

pattern

identified

as

"CRAB

carbon and oxygen as the predominant elements,

evidenced by energy peaks in the 0.2 keV and 0.5

keV regions, respectively, corresponding to the

K series. The analysis revealed the elemental

composition of the sample, with carbon (60.34%)

and oxygen (59.06%) being the predominant

elements. Other elements such as sodium,

magnesium, aluminum, silicon, phosphorus,

potassium, calcium, titanium, and iron were

present in smaller quantities. The relative atomic

fraction percentages further confirm a uniform

distribution of these elements within the sample,

suggesting a well-distributed composition.

NANOSILICA" distinctly features a prominent

peak at approximately 22° on the 2θ scale,

reflecting a high concentration of silica in

nanostructured form. The accompanying minor

peaks further suggest structural complexity and

multiphase composition, characteristics typical

of biologically derived materials and chemically

synthesized composites. These findings are

consistent with anticipated structural attributes

for silica-mineral composites sourced from crab

exoskeleton waste.

Moreover, the XRD spectrum exhibits several

minor peaks distributed across the entire range,

indicating the coexistence of multiple crystalline

phases alongside possible amorphous structures

within the material. The presence of these

diverse phases emphasizes the significance of

crystallinity in achieving the desired physical

and chemical properties of nanosilica and

related mineral compounds derived from crab

exoskeletons.

The findings indicate that the sample primarily

consists of carbon and oxygen, which together

represent a substantial portion of the total

weight. Additionally, the presence of silicon,

which constitutes 5.03% of the sample's weight,

is particularly noteworthy. This suggests that

the material may share similarities with silicon-

containing compounds, such as silicates, likely

due to the applied synthesis processes.

Figure 6. Structural composition of crab nanosilica

Figure 5. Composition of crab nanosilica

XRD Test

Transmission Electron Microscopy (TEM)

• Crab nanosilica

The TEM images presented in Figure 7 (a)-

(b)-(c)-(d) confirm the successful synthesis

of materials exhibiting typical nanometric

structures, characterized by agglomerations and

morphological variations.

Figure 6 presents the XRD analysis illustrating

a

diffraction pattern typical of nanosilica

synthesized from crab exoskeletons.

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Table 3. Quantity of Specimens for the Compression Strength Test.

In Figure 7A, a small agglomeration of particles

with irregular morphology is observed. The

variations in contrast suggest differences in

thickness or density, indicating the coexistence

of both large and small structures within a

more uniform matrix. Figure 7B displays a large

agglomeration of particles with a dense and

complex structure. The irregular shape and

regions of greater opacity imply the presence

of multiple layers or phases in the material,

suggesting potential interactions between the

particles and the matrix. Figure 7C depicts a

more compact agglomeration of particles with

well-defined edges, suggesting a higher degree

of structural organization within the sample.

The structure exhibits an irregular morphology

with a uniform opacity distribution, indicating

consistency in material synthesis.

Mix

Name

Number of

Specimens

No.

Description

Test

1

M

M+S_0.25%

C

Standard Mix

30

Standard Mix + 0.25%

2

3

4

30

Simple

Compressive

Strength.

Nanosilica

Standard Mix

30

Standard Mix + 0.25%

C+S_0.25%

30

Nanosilica

Total

120

Table 4. Quantity of Specimens for the Permeability Test.

Mix

Name

Number of

Specimens

No.

Description

Test

1

M

Standard Mix

1

Standard Mix + 0.25%

Nanosilica

Standard Mix

Standard Mix + 0.25%

Nanosilica

Permeability

2

3

4

M+S_0.25%

C

1

C+S_0.25%

Total

4

In contrast, Figure 7D presents

a

small

agglomeration of particles with a simpler and

less dense structure compared to Figure 7B.

The variations in contrast suggest differences in

composition or particle thickness, indicating a

well-distributed composite structure.

Methodological Design

The experimental methodology adopted in

this study follows the guidelines established

by INEN standards to guarantee precision and

reproducibility in mortar and cement testing

through systematically standardized protocols.

Particularly, NTE INEN 2518 outlines optimal

practices related to material proportioning and

mixingprocedures,ensuringconsistentandreliable

test outcomes. The correct dosage is verified using

containers of known volume, with sand quantities

adjustedasneededtomaintainmortarconsistency.

To ensure homogeneity, the recommended

procedure involves initially combining most of the

water with a portion of the sand and cementitious

materials rapidly and uniformly. Subsequently, the

remaining components are gradually introduced

into the mixture. Additionally, the standard

prescribes a mixing duration of between 3 and

5 minutes after the final addition of water. The

methodology also includes a retempering step to

compensate for water loss through evaporation,

thus preserving the mortar's required workability

prior to application in construction processes (28).

The observed contrast variations among the

particles correspond to nanoscale topographical

differences, typically encountered in advanced

materials synthesized via chemical or mechanical

routes. Such nanoscale features are especially

significant in applications requiring enhanced

electrical conductivity and extensive surface

area, including flexible electronic components

and supercapacitor technologies.

Additionally, the procedure requires precise

determination of material proportions, as outlined

in Table 5. These proportions are essential for the

proper preparation of specimens, which are critical

in the design and evaluation phases of mortar

production. Ensuring accurate material ratios

enhances the reliability of test results, validating

the performance and consistency of the mortar

formulations.

Figure 7. Nanometric composition of crab silica

66

INFLUENCIA DE LA NANOSÍLICE EXTRAÍDA DE CAPARAZONES DE CANGREJO EN LAS

PROPIEDADES FÍSICO-MECÁNICAS DE LOS MORTEROS DE CEMENTO

Alvansazyazdi, Logacho, Molina, Santamaría, Cadena, Bonilla, Lascano, Bucheli, Soledispa, Crespo, Oleas, Jiménez, Espinoza, Martial, Heredia, Tapia

Table 5. Quantity of materials used for preparing 6 specimens

upon hardening. Additionally, the drop test

Fine

Aggregate

Cement

Water Nanoparticles

effectively predicts the resistance of cementitious

materials to penetration by liquids, such as water

and aggressive chemical agents, establishing it as

an essential criterion for durability assessment in

concrete and mortar applications (30).

Mix

Name Ratio

W/C

g

-

M

0.625 500.0

M+S_0.25%0.625 498.7

0.584 500.0

C+S_0.25%0.584 498.7

1596.2

312.5

292.0

1.3

-

C

1.3

Lower contact angles indicate higher wettability,

which corresponds to greater permeability. This

relationship occurs because smaller contact

angles facilitate the spreading of liquid—

typically water—over the mortar surface, thus

enhancing its ability to penetrate the material’s

microstructure (29). Hence, the contact angle is

critical in distinguishing between hydrophobic

and hydrophilic surfaces, offering insights into

the effectiveness of surface modifications applied

to nanosilica particles (8).

M: Control mortar mix with “Maestro cement”

containing 0% nanoparticles.

M+S

:

Control

silicon

mortar

mix

with^0.25%0.25%

nanoparticles.

C: Control mortar mix with “Campeón” cement

containing 0% nanoparticles.

C+S0.25%: Control mortar mix with 0.25% silicon

nanoparticles.

III. RESULTS

Uniaxial compressive strength

The mortar mixes were formulated while

maintaining a constant w/c ratio; however, the

nanoparticle content was adjusted based on

percentages relative to the cement weight, as

detailed in Table 3.

This test is among the most widely used methods

for evaluating the compressive strength of mortar.

It is typically conducted using mortar cubes,

commonly with dimensions of 50 mm, to assess

the material’s capacity to resist compressive

loads. The INEN 488 standard is frequently

utilized as the reference methodology for this

assessment (30).

The formulation and proportioning of mortar

constitute essential stages involving meticulous

selection of materials, precise mixing procedures,

and rigorous testing protocols. Mortar quality

significantly influences the durability and

functionalperformanceofmasonryconstructions.

By adhering to the specified methodology,

mortars are designed to meet established

standards tailored to particular applications,

ensuring an optimal combination of mechanical

strength and adequate workability.

Table 6 summarizes the compressive strength

results obtained for the different mortar

mixtures evaluated, recorded across multiple

curing periods. These data provide insight into

the mechanical performance evolution of each

formulation over time.

Table 6. Summary of Compressive Strength of Mortars.

Permeability Test

Drop Method

24 hours 3 days 7 days 28 days 56 days 90 days

Mix Name

MPa

1.11

1.13

4.12

5.21

MPa

3.00

2.94

MPa

4.85

4.31

MPa

6.55

6.45

MPa

7.16

MPa

7.88

M

M+S_0.25%

C

Several investigations have employed drop

tests to evaluate permeability properties in

mortars concretes (29); for example, studies

utilizing contact angle measurements have been

conducted to examine the wettability of mortar

constituents, including cement and aggregates.

Their results demonstrated that the contact

angle directly correlates with the absorption

characteristics of these granular materials,

significantly affecting critical mortar properties

such as workability and mechanical performance

7.52

8.13

12.41 15.90 23.67

28.36

28.57

31.63

31.22

C+S_0.25%

12.74 15.76 24.00

Table 6 illustrates the evolution of compressive

strength in mortar mixes incorporating nanosilica

(S₀.₂₅%), compared to conventional mixes (M and

C) across different curing periods, ranging from

24 hours to 90 days.

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Número 34 Vol.1 (2025)

Among the tested formulations, the C+S₀.₂₅% mix

consistently exhibited the highest compressive

strength at all curing ages, reaching 31.22 MPa

at 90 days, which represents a slight increase

relative to the unmodified C mix (31.63 MPa).

In the case of Type N cement, the nanosilica-

modified mix (M+S₀.₂₅%) demonstrated superior

long-term performance, achieving a compressive

strength of 8.13 MPa at 90 days, reflecting a 3.2%

improvement compared to the reference mix (M:

7.88 MPa).

Figure 8. Compressive Strength vs Time – “Campeón” Cement

The observed early-age strength development

(between 24 hours and 7 days) in the C+S₀.₂₅%

mix suggests a favorable interaction between

nanosilica and cement hydration products,

resulting in matrix densification and enhanced

particle cohesion. These findings confirm that the

incorporation of nanosilica contributes to higher

compressive strength and long-term durability,

establishing it as an effective nanomaterial

for optimizing the mechanical performance of

cement-based mortars.

Figure 9 illustrates the compressive strength

evolution of mortars prepared with Campeón

Cement, comparing the reference mix (C) and

the modified mix incorporating 0.25% nanosilica

(C+S₀.₂₅%) over various curing periods (24 hours

to 90 days).

During early curing stages (24 hours to 7 days),

both formulations exhibit similar trends with

minor variations, suggesting that nanosilica does

not significantly impact the initial hydration

process. However, beyond 28 days, the C+S₀.₂₅%

mix shows a gradual increase in compressive

strength, reaching 31.22 MPa at 90 days, which

represents a slight decrease compared to the

unmodified mix (31.63 MPa).

Compressive Strength Analysis Against Time

Figure 8 depicts a comparative analysis of the

compressive strength development over time

for mortar samples formulated with “Campeón”

Cement, evaluating differences between the

reference composition (C) and the modified

mixture incorporating 0.25% nanosilica (C+S₀.₂₅%)

over various curing ages (24 hours to 90 days).

The mechanical behavior at later curing ages

indicates that nanosilica enhances hydration

reactions, matrix densification, and particle

cohesion, contributing to greater durability

and long-term strength stability. These findings

confirm that nanosilica improves the long-

term compressive strength and durability of

cementitious materials, reinforcing its potential

At early curing stages (24 hours to 7 days),

both formulations exhibit comparable strength

development, suggesting that nanosilica does

not significantly influence the initial hydration

process. However, from 28 days onwards, the

C+S₀.₂₅% mix demonstrates a gradual increase in

compressive strength, surpassing the reference

mix and reaching 31.22 MPa at 90 days,

representing a slight improvement compared to

the unmodified C mix (31.63 MPa).

as

a

viable additive for high-performance

construction applications.

This trend indicates that nanosilica contributes

to the enhancement of microstructural integrity

within the cementitious matrix, leading to greater

durability and improved long-term mechanical

performance. These results verify that the

incorporation of nanosilica significantly improves

compressive strength and matrix densification,

supporting its suitability as an effective additive

in the development of high-performance cement-

based materials.

Figure 9. Evolution of Compressive Strength – “Campeón” Cement

Figure 10 presents a comparative analysis of

compressive strength for mortars made with

Maestro Cement (M) and a mortar incorporating

0.25% nanosilica (M+S₀.₂₅�), evaluated at curing

68

INFLUENCIA DE LA NANOSÍLICE EXTRAÍDA DE CAPARAZONES DE CANGREJO EN LAS

PROPIEDADES FÍSICO-MECÁNICAS DE LOS MORTEROS DE CEMENTO

Alvansazyazdi, Logacho, Molina, Santamaría, Cadena, Bonilla, Lascano, Bucheli, Soledispa, Crespo, Oleas, Jiménez, Espinoza, Martial, Heredia, Tapia

periods of 24 hours, 3, 7, 28, 56, and 90 days. At

early curing ages (24 hours to 7 days), both mortar

formulations exhibit comparable performance,

indicating that nanosilica does not significantly

influence the initial hydration process. However,

from 28 days onwards, the M+S₀.₂₅% mix

demonstrates superior compressive strength

compared to the reference mix, attaining 8.13

MPa at 90 days, which represents a slight increase

relative to the M mix (7.88 MPa). The improved

mechanical performance observed at later ages

suggests that nanosilica contributes to matrix

densification and enhanced particle cohesion,

ultimately leading to greater long-term durability.

These findings confirm that nanosilica promotes

the progressive development of compressive

hydration

and

improved

microstructural

these

densification.

Consequently,

characteristics lead to superior durability and

enhanced long-term mechanical integrity. The

results thus confirm nanosilica's effectiveness

in elevating the long-term compressive strength

of mortars, validating its potential as a valuable

additive for improving cementitious materials

within sustainable construction contexts.

strength,

establishing

it

as

an

effective

nanomaterial for enhancing the mechanical

properties of cement-based mortars.

Figure 11. Evolution of Compressive Strength – “Maestro” Cement

Scanning Electron Microscopy (SEM)

SEM micrographs reveal a densely compacted

granular

microstructure

with

uniformly

distributed particles of diverse sizes. This

homogeneous particle arrangement indicates

reduced porosity, a key attribute enhancing the

mechanical integrity and long-term durability of

the material.

Figure 10. Compressive Strength vs Time – “Maestro” Cement

Figure 11 illustrates the progression of

compressive strength in mortars formulated

with Maestro Cement, comparing a control

mixture (M) with a mixture containing 0.25%

nanosilica (M+S0.25%). Results indicate that the

inclusion of nanosilica consistently enhances

compressive strength at advanced curing ages

(28, 56, and 90 days)

Figure 12. Morphology and topography of type N cement mixtures

with Crab Nanoparticles.

During early curing ages (24 hours to 7 days),

both mixes exhibit similar trends with minor

variations, suggesting that nanosilica does

not significantly influence initial strength

development. However, beyond 28 days, the

• M+S₀.₂₅�:

Nanosilica

reactivity,

exhibits

facilitating

high

the

pozzolanic

formation of additional C-S-H gel, which

enhances both mechanical strength and

durability.

M+S₀.₂₅% mix demonstrates

a

progressive

increase in compressive strength, reaching 8.13

MPa at 90 days, indicating a slight increase

relative to the reference sample (7.88 MPa).

A comparable analysis was performed on

mixtures containing Campeón cement, revealing

significant densification improvements and

porosity reduction attributed to the incorporation

of nanomaterials.

The enhancement in compressive strength

observed at advanced curing periods suggests

that nanosilica facilitates more effective cement

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Número 34 Vol.1 (2025)

Figure 13. Morphology and topography of type HS cement mixtures

with Crab Nanoparticles.

• C: Displays a heterogeneous microstructure

with particles of varying sizes, a typical

characteristic of cementitious mixtures.

• C+S₀.₂₅�: The uniform dispersion of

nanosilica enhances the formation of C-S-H

gel, leading to improved strength and

durability of the concrete.

Figure 14. Nanometric Composition of mixtures.

• Base Samples M and C: A loosely packed

and porous microstructure, indicating

low particle cohesion and diminished

mechanical strength.

Transmission Electron Microscopy (TEM)

TEM micrographs provide detailed information

regarding the atomic-scale distribution within

nanomaterials, allowing precise characterization

of their structural composition, ranging from 5 µm

to 200 µm. These images reveal a more uniform

dispersion of particles and a notable decrease in

porosity. The resulting denser and more compact

microstructure indicates enhanced durability and

greater long-term resistance to both mechanical

stress and environmental factors.

The nanometric structure observed through TEM

is presented in Figure 14 and Figure 15, evidencing

matrix densification and enhanced particle

cohesion due to nanosilica incorporation

Figure 15. Nanometric Composition of mixtures with Crab Particles.

70

INFLUENCIA DE LA NANOSÍLICE EXTRAÍDA DE CAPARAZONES DE CANGREJO EN LAS

PROPIEDADES FÍSICO-MECÁNICAS DE LOS MORTEROS DE CEMENTO

Alvansazyazdi, Logacho, Molina, Santamaría, Cadena, Bonilla, Lascano, Bucheli, Soledispa, Crespo, Oleas, Jiménez, Espinoza, Martial, Heredia, Tapia

• M+S₀.₂₅� and C+S₀.₇₅�: A highly compact

and cohesive microstructure, resulting in a

significant reduction in porosity.

Permeability

Figure 18 presents the contact angle analysis for

mortars prepared with Campeón Cement (A) and

Campeón Cement modified with 0.25% nanosilica

(C+S₀.₂₅%) (B).

X-Ray Diffraction (XRD)

XRD analysis facilitates the identification and

validation of crystalline phases present in the

mixtures.

A slight reduction in the contact angle is observed

in

the

nanosilica-modified

mix,

indicating

increased wettability and higher water absorption

compared to the reference mixture. This suggests

a moderate decrease in the hydrophobicity of the

cementitious matrix, which may influence porosity

and permeability against aggressive agents.

The XRD patterns of the modified mixtures are

shown in Figure 16 and Figure 17, confirming

the presence of additional crystalline phases

associated with C–S–H formation.

• Samples with nanosilica:Higher presence of

crystalline phases and pozzolanic reactivity,

reinforcing material strength and stability.

These findings indicate that while nanosilica

enhances mechanical properties, its effect on

surface hydrophobicity can vary depending on

cement composition and curing conditions.

However, the nano-filler effect of nanosilica

contributes to matrix densification, which

may still lead to improved long-term durability

and resistance to degradation in cementitious

materials. Additionally, the particle dispersion

properties of nanosilica can optimize hydration

reactions, potentially enhancing the structural

integrity of mortar under diverse environmental

conditions.

Figure 16. Nanometric composition of mixtures of type N cement.

• M+S₀.₂₅�: A Multiple additional peaks

identified between 40º and 50º (2θ),

indicating an increased presence of

crystalline phases. Nanosilica enhances

pozzolanic reactivity, improving structural

cohesion and material strength.

Figure 18. Permeability Assessment Using the Drop Method Test –

“Campeón” Cement

Figure

19

illustrates

the

contact

angle

measurements obtained using the drop method on

various mortar samples modified with nanosilica,

compared to a reference cement sample. The

contact angle serves as a key parameter for

assessing surface hydrophobicity, reflecting the

material’s ability to repel water.

Figure 19 presents a detailed contact angle

Figure 17. Nanometric composition of mixtures of type HS cement.

analysis comparing Maestro Cement (A) with

• C+S₀.₂₅�: Multiple well-defined peaks

detected between 28º and 50º (2θ),

suggesting a higher presence of crystalline

phases and better structural organization.

Nanosilica promotes the formation of

additional hydration products, enhancing

mechanical strength.

the

nanosilica-modified

Maestro

Cement

0.25% nanosilica (M+S₀.₂₅%) (B). The nanosilica-

enhanced sample demonstrates a significant rise in

contact angle compared to the reference cement,

reflecting increased hydrophobicity and reduced

water absorption. This finding indicates that the

inclusion of nanosilica effectively improves the

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water-repellent characteristics of the mortar,

thereby potentially lowering permeability and

enhancing its resistance against moisture-induced

deterioration.

The results indicate that all mixtures exhibit

hydrophobic surfaces, suggesting low water

absorption. However, the Campeón Cement mix

with 0.25% nanosilica (C+S₀.₂₅%) records the lowest

contact angle (104.1°) compared to the reference

mix (107.5°). This slight reduction implies a minor

decrease in water repellency, potentially leading to

increased permeability relative to the unmodified

cementitious matrix.

These results verify nanosilica's role as a

hydrophobic modifier, effectively minimizing water

interaction with the cement matrix. Such behavior

likely enhances material durability by restricting

moisture penetration, which is especially beneficial

for structures subjected to harsh environmental

exposure. Moreover, nanosilica incorporation may

also strengthen adhesion and cohesion within the

cementitious matrix, further improving mechanical

performance over extended periods.

These findings suggest that while nanosilica

improves mechanical properties, its effect on

surface hydrophobicity is minimal. Nevertheless,

its matrix densification effect may still contribute

to long-term durability and resistance to

environmental degradation. The decrease in

contact angle suggests a moderate increase

in wettability, which could impact capillary

absorption. Further analysis is required to

determine its influence on moisture resistance

and performance under aggressive environmental

conditions.

Figure 19. Permeability Assessment Using the Drop Method –

“Maestro” Cement

Sustainability Analysis

Table 7 summarizes the permeability test results

obtained using the drop method for the four

mortar samples, emphasizing the impact of

different nanoparticles on the material's behavior

and performance.

The reduction of CO₂ emissions associated with

the utilization of nanoparticles derived from crab

waste was evaluated. In Ecuador, approximately

8.0 tons of crab waste are generated annually,

contributing to an estimated 3,856 tons of CO₂

emissions.

Table 7. Contact Angle Measurement.

Mix Type

M

Contact Angle

108.3°

Surface Type

Hydrophobic > 90°

An analysis was conducted to assess the CO₂

emissions resulting from the production of

mortars incorporating these nanoparticles, aiming

to quantify their potential environmental benefits

in terms of carbon footprint reduction.

Hydrophobic > 90°

M+S_0.25%

C

105.0°

107.5°

C+S_0.25%

104.1°

. CO₂Emissions Associated with Crab Waste

Mortar components

Price

TOTAL

CO₂from Decomposition % CO₂Emissions

Chemical produc-

tion

Crab waste

flour

Chemical process

CEMENT

$/kg

kg CO₂

%

Nanosílica

418.4

167

504

900

1571

3856

41%

Table 8. Sustainability Assessment and CO₂ Emissions Associated with Crab-Derived Nanosilica.

Environmental Impact of Nanomaterials

• Nanosilica derived from crab waste

contributes to a 41% reduction in CO₂

emissions.

The sustainability analysis (Table 8) shows a 41%

reduction in CO₂ emissions resulting from the use

of nanosilica derived from crab shell waste.

The chemical production process and mortar

components, including cement replacement,

72

INFLUENCIA DE LA NANOSÍLICE EXTRAÍDA DE CAPARAZONES DE CANGREJO EN LAS

PROPIEDADES FÍSICO-MECÁNICAS DE LOS MORTEROS DE CEMENTO

Alvansazyazdi, Logacho, Molina, Santamaría, Cadena, Bonilla, Lascano, Bucheli, Soledispa, Crespo, Oleas, Jiménez, Espinoza, Martial, Heredia, Tapia

significantly lower the carbon footprint compared

to conventional materials.

Future studies should focus on assessing the

performance of these mortars under more

severe exposure conditions, as well as analyzing

the interaction of nanosilica with other additives

and supplementary materials, to broaden its

application range and ensure consistent long-

term performance.

Thefindingshighlightabeneficialeffectonreducing

greenhouse gas emissions, thereby promoting

circular economy principles through the recycling

of waste materials within the construction

sector. This strategy simultaneously advances

environmental sustainability and enhances the

mechanicalpropertiesofcementitiouscomposites.

V. CONCLUSIONS

Nanosilica demonstrates superior long-term

efficiency, contributing significantly to the

mechanical enhancement of mortar over extended

curing periods.

IV. DISCUSSION

The results obtained demonstrate that the

incorporation of nanosilica synthesized from

crab shells has a positive effect on the physical–

mechanical properties and durability of the

evaluated cement mortars. The addition of

0.25% nanosilica by cement weight produced

significant increases in compressive strength,

particularlyatearlyages, whichisassociatedwith

the acceleration of cement hydration and the

formation of a denser and more homogeneous

cementitious matrix. This behavior is consistent

with findings reported in the literature on the

use of silica nanoparticles, where their high

specific surface area acts as nucleation sites for

C–S–H gel, promoting pore filling and reducing

capillary porosity.

The incorporation of nanosilica derived from crab

shell waste not only improves mortar performance

but also serves as a sustainable strategy, aligning

with circular economy principles by repurposing

industrial byproducts and reducing environmental

impact. Compressive strength results confirm

that nanosilica-modified mortars achieve high

mechanical resistance, competing closely with

other

nanoparticle-enhanced

formulations,

ensuring structural durability.

Water absorption tests indicate that nanosilica

reduces permeability, maintaining absorption

levels below 10%, which is crucial for enhancing

moisture resistance and durability in aggressive

environments. Hydrophobicity measurements

reveal that nanosilica-modified mortars exhibit

contact angles exceeding 90°, confirming improved

water repellency, which helps mitigate corrosion

risks and chemical degradation.

Microstructural analysis through SEM and XRD

confirmed the presence of hydration products

with a more uniform distribution, as well as a

reduced amount of free portlandite, suggesting

more efficient consumption of the available

calcium hydroxide. Additionally, permeability

tests and contact angle values greater than

90° confirmed a hydrophobic behavior, which

contributes to reduced water absorption and,

consequently, greater material durability against

aggressive agents.

The obtained results confirm that nanosilica meets

the requirements of the NTE INEN 2518 standard,

validating its technical feasibility for integration

into high-performance structural applications.

Future research should explore alternative sources

of nanosilica from biological waste, optimizing its

processing methods to enhance its efficiency and

applicability in sustainable construction. The use

of nanosilica in mortar formulations contributes

to reducing cement consumption, lowering CO₂

emissions, and fostering the development of eco-

friendly construction solutions.

From a sustainability perspective, the utilization

of biological waste as a raw material for obtaining

nanosilica represents a viable alternative aligned

with the principles of the circular economy,

reducing the carbon footprint and minimizing

the environmental impact associated with the

production of construction materials. However,

it is recognized that variability in the chemical

composition of the waste and the need to

optimize synthesis processes may influence the

reproducibility of the results.

Overall, nanosilica proves to be

a

viable

nanomaterial for improving mechanical strength,

water resistance, and long-term performance

in cementitious composites, reinforcing its

73

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Número 34 Vol.1 (2025)

importance in sustainable and high-performance

construction applications.

project. We also extend our thanks to the staff of

the Ecuadorian Institute of Cement and Concrete

(INECYC) for their collaboration in conducting

specialized tests. Likewise, we are grateful to the

laboratories of Material Testing and Chemical

Sciences at the Central University of Ecuador (UCE)

for their commitment and professionalism in the

sample analysis. Finally, we express our gratitude

to the Ministry of the Interior for their support,

which was essential for the successful completion

of this research.

VI. ACKNOWLEDGEMENTS

We would like to express our deepest gratitude to

theNanoscienceandNanotechnologyCenterofthe

Armed Forces University (ESPE) and its laboratory

team for their valuable technical support and

dedication throughout the development of this

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PROPIEDADES FÍSICO-MECÁNICAS DE LOS MORTEROS DE CEMENTO

Alvansazyazdi, Logacho, Molina, Santamaría, Cadena, Bonilla, Lascano, Bucheli, Soledispa, Crespo, Oleas, Jiménez, Espinoza, Martial, Heredia, Tapia

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