Construction and Building Materials 362 (2023) 129767

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Construction and Building Materials

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

Investigation on fluidity, microstructure, mechanical and durability

properties of snail shell based graphene oxide cement composite material
Suseela Alla *, S.S. Asadi
Department of Civil Engineering, Vignan’s Foundation for Science, Technology and Research, Vadlamudi, Guntur 522213, A.P, India

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

Keywords: In recent years, there has been a more usage of Graphene Oxide nanomaterial to enhance the desirable qualities
Cement of cement-based composites. The fluidity of cement composites and the workability of concrete, on the other

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Snail shell powder hand, may be lowered as a result of the introduction of graphene oxide (GO). In this research, a simple and
Graphene oxide (GO)
inexpensive additive snail shell powder was employed to increase the fluidity of graphene oxide cement com­
Fluidity
Microstructure (SEM)
posites. Additionally, the microstructure, mechanized, and durableness performance of snail shell (SS) based
Strength and durability graphene oxide (GO) cement composites was studied. Snail-Shells are examples of bio-shell debris that is wasted
from restaurants and the seas every day. Because of poor maintenance of waste, SS are deposited as rubbish on
vacant areas and in landfills. The snail shell powder has a spherical shape and has a pozzolanic character, similar
to that found in cement. In the current study, snail shell powder was employed in GO-cement composites to
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substitute a portion of the cement, and the performance of the composite material’s fluidity, microstructure,
mechanical, and durability characteristics were investigated. The impact of snail shell powder was investigated
at 10 wt%, 15 wt%, and 20 wt%, replacement of cement, with graphene oxide (GO) addition ranging from “0.01
wt%, 0.02 wt%, 0.03 wt%, and 0.04 wt%”. The amount of snail shell powder added to the GO composite
enhanced the fluidity. A result of the reduced water requirement, the spherical form of the snail shell powder
(SSP) and the pozzolanic nature of the SSP, the improved fluidity of the GO-cement composite was obtained. The
SEM examination were used to establish the micro structural study of the cement composite. In the SEM pictures,
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it could be shown that the combination of SS and GO changed the nature of structure of the composite from one
that was porous to one that was significantly pore filled, resulting in better mechanical and durability charac­
teristics. At 3, 7, and 28 days of curing, snail shell based GO-cement composites demonstrated stronger
compressive and flexural strengths than the control sample, despite the fact that the snail shell powder dose was
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less than 20 % of the total weight of the cement. Finally, the inclusion of snail shell powder material to the GO-
cement composite resulted in an excellent solution to the fluidity issue that had been encountered.

1. Introduction Ettringite (AFt), and Calcium Hydroxide (Ca (OH)2, CH)” promote
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brittleness in cement composites [5].

The use of cement in the building sector has increased in recent
years. It has remarkable bonding and strength properties when applied
to concrete constructions. Although cement has several advantages in
concrete constructions, it also has detrimental environmental conse­
quences [1,2]. Because cement making uses a lot of energy. Regardless
of energy, “a huge amount of CO2 is discharged into the environment.
Thus, limiting cement consumption reduces CO2 emissions [3]. The
cement industry has been emitting roughly 0.83 kg of CO2 per kilo­
gramme of cement, with a 12 % global discharge by 2020 [3,4]. The
brittleness of cement causes fissures in concrete constructions. Hydra­
tion products such as Calcium Silicate Hydrate Gel (C–S–H Gel),
Composites made of cement have excellent compressive but low
flexural strength. Fibers are often utilised in cement composites to in­
crease flexural strength [4]. However, using fibres did not reduce brit­
tleness, resulting in cracks in composites of cement. So, fibres in
composites couldn’t boost flexural strength. Modern concrete requires
high performance structural engineering materials with high fluidity,
homogeneity, and viscosity to avoid aggregate segregation, maintain
concrete stability until hardened, and improve flexural performance.
This is because nanomaterials like SiO2, TiO2, ZnO, CNT and GO have
recently emerged in construction materials to obtain greater strength
qualities [6,7]. Many waste items and industrial byproducts may be

* Corresponding author.

https://doi.org/10.1016/j.conbuildmat.2022.129767
Received 19 April 2022; Received in revised form 6 July 2022; Accepted 13 November 2022
Available online 19 November 2022
0950-0618/© 2022 Elsevier Ltd. All rights reserved.
S. Alla and S.S. Asadi
utilised to manufacture concrete in place of cement, for example, Red
mud, fly ash, snail shells, clamshells, and glass may all be utilised
[8–10].
Graphene oxide (GO) has the best strength, surface area, and aspect
ratio of among all nanomaterials [11]. With “hydroxyl epoxide func­
tional groups on its base planes and carbonyl and carboxyl groups on its
sheet edges, it was stronger and more durable” [5,12,13]. GO dispersed
in water with 1-nm thick sheets is simple with oxygen-containing
functional groups [11]. This graphene oxide nanomaterial has a 130
MPa elastic modulus [14,15]. It is frequently manufactured in bulk from
cheaper graphite powder. Graphene oxide may be used to strengthen
cement composites, overcoming problems with cement composites. The
addition of GO to the cement paste lowered the fluidity and workability
by raising the viscosity [16–18]. In this case, more water is needed than
the w/c ratio indicates to increase fluidity. The additional water may
reduce the strength.
To increase the fluidity of GO-cement composites, snail shell powder
is used as a cheap additive. Restaurant and marine garbage snail shells.
Snail shells litter idle ground due to poor waste management. In com­
parison to cement, snail shell powder requires less water and is spherical
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in form. The pozzolanic properties of snail and clamshells to manufac­
ture cement composites with a cement content of 0 % to 30 % [19].
Maximum compressive strength is 20 MPa with 20 % snail shell ash
substitution. With 25 % calm shell ash replacement the strength is 30
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MPa. They said that the compressive strength went down with more ash
from snail and clam shells, the optimal percentages were 20 % and 25 %.
An alternative to cement [20] utilised snail shell powder instead. Using
15 % snail shell powder substitution for a curing period of 7 and 28 days
resulted in a compression strength of 21.42 Mpa and 32.52 Mpa. In this
study, a snail shell powder substitute of 10 %, 15 %, and 20 % was
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studied with graphene oxide percentages of 0.01 wt%, 0.02 wt%, 0.03
wt% and 0.04 wt% by the weight of cement. We built ordinary cement
paste composites to compare to the GO and snail shell powder com­
posites [21, 22]. The microstructure, mechanical and durability prop­
erties of snail shell-based graphene oxide hardened cement composite
was determined. Particularly, the cement composite material’s resis­
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tance to deterioration in an acidic environment is thought to be its most
important characteristic. Because of the increasing capillary gaps in
acidic conditions, cement composite materials suffer severely. Through
capillary spaces, acids may easily enter the composite structure and
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interact with the calcium hydroxide component of the cement paste.
Similar to “how calcium hydroxide (C–H or Ca(OH)2) combines with
these sulphate ions to form calcium sulphate, CaSO4⋅2H2O, in cement
composite (gypsum). Additionally, this calcium sulphate combines with
cement hydrates (tricalcium aluminate, or 3CaO.Al2O3) to create cal­
cium trisulfoaluminate, commonly known as ettringite (AFt)
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(Ca6Al2(SO4)3 (OH)12⋅26H2O). In the presence of water, AFt breaks
down into calcium monosulfoaluminate (AFm) and sulphate ions when
it combines with excess gypsum [23]. Due to temperature changes that
result in the volumetric expansion of the cementitious matrix, these
unstable substances further re-form ettringite, which is known as
delayed ettringite formation (DEF) [24]. Ettringite also plays a signifi­
cant role in cement hydration as the primary destructive compound in
sulphate attack”. Therefore, this research effort also examines the
qualities that affect the transport mechanism and chemical deterioration
of the cement composite material, such as resistance to acid attack,
resistance to sulphate attack, and resistance to chloride attack.
2. Required materials and test methods
2.1. Chemicals and materials
The materials utilised in this investigation include ordinary Portland
cement (OPC) of grade 53 from KCP Cements is accepted with “ASTM C
150–19” [25], Guntur, Andhra Pradesh. The snail shell powder
confirmed with “ASTM C 618–08” [26], and water dispersed graphene
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Construction and Building Materials 362 (2023) 129767
oxide solution (4 mg/ml concentration) from Graphenea Company,
Spain. To calculate pozzolanic materials, EDS measured the “chemical
composition of cement and snail shell powder” as indicated in Table 1,
and the calculation of pozzolanic materials includes SiO2 + Al2O3 +
Fe2O3 ≥ 40 wt%. The preliminary tests on cement and snail shell powder
resulted as specific gravity of cement and snail shell powder is 3.17 and
2.43. The specific surface area of cement and SSP resulted as 321 m2/kg
and 19,500 m2/kg. Table 2 & Fig. 1 exhibit the graphene oxide char­
acteristics. The primary functional groups on graphene oxide are –OH
and –COOH. Fig. 2 shows a SEM picture of graphene oxide.
Generally, graphene oxide is available in two forms i.e., in powder
form and colloidal water dispersion solution. Colloidal means, it is a
highly dispersed & evenly suspended material in liquid. Such that in the
chosen GO solution, the GO nano particles are highly dispersed and
evenly suspended in the water dispersed GO solution. So for convenient
mixing with cement composite, water dispersed solution was utilized in
this research work. In each graphene oxide cement composite prepara­
tion normal water was substituted with GO aqueous solution to keep the
constant or equal quantity of mixing water at all mixes of graphene
oxide cement composite specimens.
2.2. Snail shell powder preparation
Specifically, the powder made from the snail shells under consider­
ation is employed in this study. The snail shells are collected near Tenali
Coastal Area, Andhra Pradesh, India. The powder has been retrieved
from shells by grinding. The method of making snail shells powder is
shown in the following bullet points.
a. Firstly, the snail shells are collected at nearby coastal area, Andhra
Pradesh.
b. Clear all the organic matter in shells with water and keep the shells
under sun for drying.
c. Grind the shells until to get the Powder, sieve them in 90-µm and
store them in an airtight container.
The chemical composition of snail shells powder (SSP) is presented
in Table 1, while the particle size distribution of snail shell powder (SSP)
and cement is presented in Fig. 3. Fig. 4 shows the results of the XRD
examination. Aragonite (CaCO3) is the main element of SSP, and has a
high frequency of 2θ = 26◦ and 33◦ . The second fundamental ingredient
of snail shell is quartz (SiO2), which is found in varying ranges of 2θ (46,
48, 53, and 58◦ ). Portlandite (1 8 0), Quartz (24, 28◦ ), Alite (31, 33◦ ), and
Belite (35, 36◦ ), are the important peaks of cement, with additional
components detected at various ranges of 2θ in Fig. 4.
When compared to cement, SSP has high amount of silica. Micro­
structural investigations show that adding silica to sample mixtures
creates “C–S–H gel and Ettringite structures”. Fig. 5 shows a SEM
picture of SSP.
Snail shell powder exhibits spherical and needle-like shapes, as
shown in Fig. 5. Due to the evolution of heat during the hydration
process, needle structures are created from spherical shaped particles.
These needle structures aid in the formation of Ettringite in cement
composites and have an impact on their strength.
2.3. Casting and testing
The cement paste was made using a cement content of 500 g, 225 g of
water, snail shell powder, and varied amounts of graphene oxide solu­
tion distributed in water, all of which were combined to make the final
product. First, the GO solution and water were combined and then
added to the cement, resulting in the creation of the GO-cement paste.
Once the GO-cement paste had been combined for 30 s at a low speed
with a mixer, SSP was added with a focus on increasing the fluidity of the
mixture. Following that, the mixing might be maintained for another 30
s. Following that, the mixing speed may be raised to allow for another
S. Alla and S.S. Asadi Construction and Building Materials 362 (2023) 129767

Table 1
Cement and Snail shell powder chemical composition.
Chemical Constituent SiO2 Al2O3 Fe2O3 CaO MgO K2O Na2O SO3 TiO2 P2O5 Mn2O3

Cement (%) 21.65 5.95 3.18 64.89 1.8 0.97 0.61 1.95 – – –
Snail shell powder (%) 34.63 4.89 4.28 53.78 1.21 0.97 0.36 0.54 0.63 0.42 0.06

Table 2
Graphene oxide (GO) elemental analysis (www.graphenea.com).
Material Carbon Hydrogen (H) Nitrogen (N) Sulphur Oxygen
(C) (S) (O)

GO 49–56 0–1 0–1 0–2 41–50

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Fig. 1. X-ray photoelectron spectroscopy (XPS) of graphene oxide (https:
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//www.graphenea.com).
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Fig. 4. XRD Analysis of Snail shell powder.

respectively, after 3, 7, and 28 days of curing. The “ASTM C109” [27]

Fig. 2. SEM image of GO (https://www.graphenea.com).
standard was used to test the compression strength of composites.
Control specimens were also made without snail shell powder or gra­
phene oxide (GO). For the cement paste, the Water to the cement ratio
was 0.45 used. The specifications of cement paste mix proportions can
be observed in the Table 3. The fluidity and viscosity properties were
assessed through flow table test and setting time was assessed through
Vicat’s apparatus.

30 s of mixing with the mixer. Next, after mixing at high speed for 30 s,
turn off the mixer and let the cement paste to rest for 150 s before 2.4. Specimens casting and curing
blending it again. These tests were performed on specimens with di­
mensions of “70 × 70 × 70 mm; 40 × 40 × 160 mm; and 100 × 50 mm”, The casting of specimens has been done using the cast or wood

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S. Alla and S.S. Asadi Construction and Building Materials 362 (2023) 129767

2.5. Flow Table (Fluidity) test

The fluidity test is used to calculate the quality of cement composite

consistency, cohesiveness and segregation. The composite mix has been
prepared by considering the mix proportions according to Table 3. Clean
the surface of flow table along with the cone. Place the freshly mixed
sample in cone in two layers and tamp each layer with a tamping of rod
of 25 times to exhale the voids present in the composite. Lift-up the mold
slowly and let the cement composite stand on its own without any
support. Raise the table for about 1.25 cm and drop it and repeat the
same for 15 times within a period of 15 s. Measure the diameter of
spreader composite horizontally and vertically. The mean of diameter
shall be the measurement of flow ability of cement composite in “mm”.

2.6. Compressive strength and flexural strength test

These tests are carried out on cement composite specimens that are
70 mm cubes and 40 mm prisms in size, as per “I.S. 516-2013” [28]. The
casted samples were then hydrated for 3, 7 and 28 days as per “I.S.
9013–1978” [29]. The samples are tested for compressive and flexural

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strength using a 1000 kN Universal Testing Machine.

Fig. 5. SEM image of Snail Shell Powder (SSP).

2.7. Water absorption test

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After 28 days of desired curing in a water bath, the casted specimens
Table 3 of size 70 mm × 70 mm × 70 mm are used for the water absorption test
Mix Proportions. as represented in Fig. 6. As per “I.S:1199 (1959) [30]”, the samples were
Material Type Cement Snail Shell Powder (SSP) GO Water
removed and warmed up for 72 h at 100 ◦ C. After 72 h, weigh and
(%) (g) (g) aq. (g) discard the samples. W1 is the oven-dry sample weight. After taking the
(g) dry weight, keep all the samples in a tub of water for 24 h like Fig. 5.
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GO-0 SSP-0 500 0 0 225 Takeout the samples after 24 h, pat dry and weigh the samples W2.
GO-0.01 SSP-0 500 0 12.5 212.5 Water absorption is given as a percentage using Eq. (1).
GO-0.01 SSP- 450 50 12.5 212.5
10 W2 − W1
W.A (Water Absorption) (%) = *100 (1)
GO-0.01 SSP- 425 75 12.5 212.5 W1
15
GO-0.01 SSP- 400 100 12.5 212.5 where, W1 = Oven weight, W2 = Wet Weight.
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GO-0.02 SSP-0 500 0 25 200
2.8. Sorptivity test
GO-0.02 SSP- 450 50 25 200
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In this case, sorptivity is used to calculate the water penetration
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GO-0.02 SSP- 425 75 25 200

15 value. The test disc will be 50 mm thick and 100 mm in diameter is
GO-0.02 SSP- 400 100 25 200
accepted with “ASTM C 1585-20” [31]. Except for the water-facing side,
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GO-0.03 SSP-0 500 0 37.5 187.5
all disc surfaces are non-absorbent, like silica gel. Fig. 7 shows the setup
GO-0.03 SSP- 450 50 37.5 187.5 of Sorptivity test. First, the exposure’s side water penetration is esti­
10 mated over time. To get Sorptivity values, Eq. (2) was utilized.
GO-0.03 SSP- 425 75 37.5 187.5
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15 i
S = √̅ (2)
GO-0.03 SSP- 400 100 37.5 187.5 t
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GO-0.04 SSP-0 500 0 50 175 “Where S = Sorptivity (mm/min0.5), i = A*d Δw
, ∇W = Weight of sam­
GO-0.04 SSP- 450 50 50 175 ples concerning time, d = density of water, t = Elapsed time in minutes,
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GO-0.04 SSP- 425 75 50 175
15
GO-0.04 SSP- 400 100 50 175
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molds. The molds are greased with lubricants like mud oil or grease to
facilitate easy de-molding. The basic materials for cement composite are
weighed and measured. All the materials of composite are kept in metal
tray and mix together until to get the homogeneous mix. Place the mixed
material in molds with three layers arrangement and place the molds in
vibrating machine to remove the air voids present in composite. Keep
the molds for 24 h to get the composite hard and remove from molds
after 24 h. The removed composite samples are now placed in water bath
with a required curing period. At least 3 samples for each mix have been
casted for a curing period of “3 days, 7 days, and 28 days”. Fig. 6. Setup of Water Absorption.

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S. Alla and S.S. Asadi Construction and Building Materials 362 (2023) 129767

Table 4
RCP Test Values (“ASTM C1202-12 (2012)” [32]).
Charge (Coulombs) Chloride Permeability

>400 High permeability is high

2000-4000 Medium permeability
1000-2000 Permeability is low
100-1000 Permeability is very low
<100 Negligible permeability

which is presented in Fig. 9. Takeout the samples from acid bath after 28
days of immersion, wipe off the surfaces with cotton cloth before testing.
There was a change in mass, compressive strength, and diagonal di­
mensions. The factors of loss of mass, acid attack, and loss of strength
factors were determined and which are confirmed with “ASTM C
666–1997 [33]” for snail shell-based graphene oxide cement composite
specimens. Durability Loss in specimens in terms of strength, mass and
dimensions are collaborated to get a Unified Factor termed as Acid
Durability Loss Factor.
Fig. 7. Sorptivity test setup.
a) Acid mass loss Factor (AMLF)

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and A = area of the disc”.
By immersing the cubes in acid solutions and finding the mass in a
specific time period, the percentage of loss of mass loss is evaluated. The
2.9. Rapid chloride permeability test mass change with age is determined as the Acid mass loss factor which is

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depicted with actual mass of all sample (AMLF) has been calculated by
To electrical conductivity of composite have been evaluated and are using Eq. (4).
confirmed with, “ASTM C1202-12 [32]” employed by the RCP test. The
final discs are 50 mm high and 100 mm in diameter. Both negative and AMLF =
Mass of sample treated with Acid
× 100 (4)
positive RCP Test cells with “3% NaCl and 0.3 M NaOH” were used to Actual mass of sample
test the specimens. Fig. 8 shows the RCP Test sample setup. Coulombs of
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Eq. (3) can compute electricity flow between two reservoirs. b) Acid Attacking Factor (AAF)
Q = 900 × 10-3 [(I0 + I360) + 2(I30 + I60 + I90 + ….…............ + I300 + I330)]
(3) The degradation was measured at each diagonal of the face from
opposite side. The change in diagonal length after a specific duration in
The RCP Test values correspond to Table 4 values. “ASTM C1202-12 the acid is specified as the Acid Attacking Factor (AAF) evaluated using
[32]” reaffirms them. According to Table 4, lower permeability means Eq. (5) [34], [35].
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reduced charge flow (coulomb) and higher resistance.

Dimensional Change of Sample Treated with Acid
AAF = × 100 (5)
Actual Dimension of Sample
2.10. Acid durability test
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c) Acid strength loss Factor (ASLF)

After 28 days, the samples of size 70 mm × 70 mm × 70 mm casted
and cured are collected and dried for 72 h at 100 ◦ C. Removing samples
After immersion in acid the relative strength in concrete specimens is
from oven, note their mass, strength, and diagonal dimensional values.
Then, three specimens from each batch were immersed in 2 and 5 % of Acid strength loss factor (ASLF) which is calculated using Eq. (6). The
relative strengths of the compressive strength measurements are always
sulfuric acid (H2SO4) and hydrochloric acid (HCl) acid mixtures with a
compared to 28 days [34].
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pH of 0.3. The samples are kept in the acid solution at about 28 days

Fig. 8. RCP Test setup of samples. Fig. 9. Suspension of Samples in Acid Solution.

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S. Alla and S.S. Asadi
Strength change of sample treated with Acid
ASLF = × 100
Actual Strength of Sample
d) Acid durability loss Factor (ADLF)
A single unified element known as “Acid durability loss factor
(ADLF)” has been established to incorporate the effect of several ele­
ments such as loss of mass, loss of strength and loss of dimension is
analyzed by Eq. (7) [34].
ADLF = AMLF × AAF × ASLF
2.11. Microstructural studies
Scanning Electron Microscope (SEM) is used to study the
morphology of cement composite samples. Scanning Electron Micro­
scope (SEM) is a test process that scans a sample with electronic beam to
produce a magnified image for analysis. From the microstructural
analysis it can be analyzed the reason for the improvement in strength
properties of hardened cement composite samples. The testing samples
are taken from hardened composite with a dimension of “10 mm × 10
mm × 5 mm” smooth composite parts. Fig. 10 depicts the Scanning
Electron Microscope (SEM) equipment used to study the microscopic
characteristics of hardened cement composite samples (Figs. 11-14).
3. Results and discussions
3.1. Consequences of GO on the workability of the cement composite
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Graphene oxide has changed the property of workability of cement
composite in form of how fluid it is, how quickly it starts to set, and how
long it takes to harden. This is shown in the Table 5. graphene oxide in
cement paste made it less fluid, more viscous, and faster to set. This was
found out from the results. Workability of cement paste has reduced a lot
when 0.04 % GO was added to the mix. In this study, it was found that
adding GO to cement may make the cement paste more viscous and
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make it easier to mix with water. Also, GO nanoparticles and hydrated
cement particles came together to form cement particles that were
grouped together. The chemical reaction between the alkaline envi­
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ronment of the cement and a large number of functional groups on the
GO surface and edges caused the cement to hydrate faster and set faster.
As a result, found that fluidity and viscosity both went down and up in
their studies [36,37]. The electrostatic interactions between GO and
cement particles produce agglomeration and clumping in cement com­
posites. Graphene oxide nanoparticles have a large surface area and are
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hydrophilic, making them less fluid [36–39].
3.2. Consequence of SSP on fluidity of GO cement composite
In this work, a simple and affordable addition of SSP was advised to
Fig. 10. Scanning Electron Microscope (SEM) equipment.
Construction and Building Materials 362 (2023) 129767
improve the fluidity of GO cement composite. The effect of SSP on GO-
(6)
cement paste fluidity was studied using a flow table. The fresh cement
paste samples are combined with 0.01 %, 0.02 %, 0.03 % and 0.04 % GO
and 10 %, 15 % and 20 % snail shell powder to make GO cement
composite. GO cement paste fluidity was tested at 5-minute, 30-minute,
60-minute, 90 min, and 120-minute intervals. Adding snail shell powder
to GO cement paste increased fluidity while increasing snail shell con­
tent. The preliminary fluidity was 255 mm at a maximum 20 % snail
shell powder substitution in GO cement paste. At all GO doses (0.01 % −
0.04 %), the fluidity loss of cement pastes without mixing the snail shell
(7) powder is quite substantial at 30 min, as shown in Figures (11, 12, 13,
and 14). When compared to the typical sample, the samples with 0.01 wt
%, 0.02 wt%, 0.03 wt%, and 0.04 wt% of GO have losses of flow of 13.3
%, 15.6 %, and 22.2 %, respectively, at 30 min. However, when SSP was
add-on to the GO-cement paste, the fluidity loss was minimized
compared to the control sample. Actually, snail shell powder particles
act as a ball bouncing between the particles of cement, reducing cement
precipitation and increasing graphene oxide-cement fluidity. This is
owing to their low water need, finer particle size than cement particles,
and spherical shape. This indicates that the addition of snail shell
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powder material decreased GO-cement particle flocculation.
3.3. The effect of SSP and GO on strength properties of cement composite
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The properties of strength were determined for the mix proportions
of GO addition at 0 %, 0.01 wt%, 0.02 wt%, 0.03 wt%, and 0.04 wt%,
with Snail Shell Powder (SSP) at 10 %, 15 % and 20 % replacement by
the weight of cement. At least 3 samples for each mix have been casted
for a curing period of “3 days, 7 days, and 28 days”. The total number of
casted cube specimens are 153 for finding the compressive strength
values of snail shell based GO-cement composite mixes; in such a way
that another 153 prism specimens were casted for finding the flexural
strength values of snail shell based GO-cement composite mixes. Ac­
cording to “the gradual increment of GO dosages from 0.01 % to 0.04 %
along with snail shell powder replacement at various percentages to the
weight of the cement, the compression and flexure strength results of
GO-Cement composite samples were increased at 3, 7 and 28 days of
curing, compared to the strength results of normal cement composite
mixes”. Among all mixes, at each GO dosage from 0.01 % to 0.04 % with
20 % snail shell powder higher strength values were achieved at 3, 7,
and 28 days of curing. Then higher strength results of those snail shell-
based GO-Cement composite mixes represented in Figs. 15 & 16 and also
the SEM analysis was done to these composite mixes for assessing the
effect of graphene oxide (GO) snail shell powder (SSP) combination on
cement composite.
The flexural strength steadily improved up to GO-0.03 %, SSP-20 %
mix percentage owing to appropriate dispersion of all hydration crystals
in void spaces and associated development of oxygen functional groups
on GO surface to hydration crystals in hardened cement composite
structures. “After 28 days of curing, the samples with (GO-0.03 %, SSP-
20 %) mix percentage had a 63.47 % increase in flexural strength
compared to the samples without graphene oxide (GO) and SSP”, and
increasing the GO dose to (GO-0.04 %, SSP-20 %) reduces the flexure
strength of cement composites as shown in Fig. 15. The compression
strength of the cement composite with (GO-0.04 wt%, SSP-20 %) mix
fraction improved by 42.6 % after 28 days of curing compared to the
samples without GO and SSP as shown in Fig. 16.
3.4. The effect of SSP and GO on durability properties of cement
composite
For evaluating the durability properties such as, “Water absorption
test, Sorptivity test, Acid resistance test and Rapid Chloride Permeability
Test” sample sizes were regarded as “70 × 70 × 70 mm cubes, 40 × 40 ×
160 mm prisms and Φ100 × 50 mm” discs were evaluated at 3, 7, and 28
days of curing time.
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S. Alla and S.S. Asadi
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Fig. 11. Cement paste fluidity with Snail Shell Powder (SSP) and GO dosage at 0.01% wt. of cement.
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Fig. 12. Cement paste fluidity with Snail Shell Powder (SSP) and GO dosage at 0.02% wt. of cement.
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3.4.1. Water absorption test
Fig. 17 shows that the resistance to water absorption decreased with
increased GO level at 0.04 % in the cement composite. The maximum
resistance was recorded at GO-0.03 % and SSP-20 % sample mixes.
Conversely, all snail shell-based GO-cement composite mixes displayed
superior water resistance compared to the traditional sample mixes. The
findings show that the GO-0.03 % and SSP-20 % sample mixes in cement
composite had the greatest reduction in water absorption after the
curing of 28 days compared to the control samples. The refinement of
the pores of composites of cement was achieved by decreasing the pore
diameter, which results in an increase in water absorption resistance of
cement composite.
3.4.2. Water sorptivity test
The maximum resistance to water sorptivity was found in the sample
mixes with GO-0.03 % and SSP-20 %, but at 0.04 % with SSP-20 %, the
resistance to water sorptivity was reduced because GO particles in the
cement composite started to get stuck together. All snail shell-based GO-
cement composite mixes were more resistant to water capillarity than
control cement mixes, and the results are represented in Fig. 18. GO-
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Construction and Building Materials 362 (2023) 129767
0.03 % and SSP-20 % sample mixes in cement composite were found to
have the best water sorptivity coefficient values at all-time spans than
the control samples.
3.4.3. Rapid chloride permeability test
The flow of chloride ions to snail shell-based GO cement composites
was studied for samples with a 28-day curing time. According to “ASTM
C 1202–12 [32]”, the charge passed in terms of coulombs through the
snail shell-based GO-cement composite samples is less compared to the
normal composite of cement samples. The cement composite samples
with SSP-20 % at 0.01 wt% and 0.02 wt% GO addition exhibited mod­
erate chloride permeability; at 0.03 wt% GO addition exhibited low
chloride permeability; and at increased GO content at 0.04 % exhibited
again moderate chloride permeability as shown in Table 6, due to the
clustering of graphene oxide nanoparticles at higher dosage of GO
addition in cement composite samples. But normal cement composite
samples with 0 % GO addition exhibited high chloride permeability,
these results represent the pore structure refinement is enhanced in the
cement composite samples due to the addition of GO nanomaterial along
with the pozzolanic property of snail shell powder material, it results in
S. Alla and S.S. Asadi Construction and Building Materials 362 (2023) 129767

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Fig. 13. Cement paste fluidity with Snail Shell Powder (SSP) and GO dosage at 0.03% wt. of cement.

TE
AC
R
ET

Fig. 14. Cement paste fluidity with Snail Shell Powder (SSP) and GO dosage at 0.04% wt. of cement.
R

between acids and the calcium hydroxide part of the cement paste,
Table 5
resulting in highly soluble calcium salts. These soluble calcium salts
Influence of GO on fresh state properties of cement composite material.
rapidly dissolve in cement paste, degrading its overall structure. The
Quantity of GO (wt. %) 0 0.01 0.02 0.03 0.04 interaction between GO nanoparticles and cement particles enlarges the
Cement paste fluidity(mm) 255 196 198 110 90 shape and size of the cement particles, allowing them to penetrate the
Initial setting time (min) 60 58 53 50 45 void spaces and enhance the void structure. As a result, acid solutions
Final setting time (min) 480 470 465 455 440 cannot penetrate into the gaps and react with the calcium hydroxide in
the cement paste.
representing the greater resistance to the chloride ion permeability in After “28 days immersion in 2 % and 5 % concentrations of both
snail shell based GO cement composite samples, which is compared to H2SO4 and HCl acid solutions”, the highest drop in Acid Durability Loss
the normal cement composite samples. Factor (ADLF) was recorded for GO-0.03 % and SSP-20 % sample mix­
tures. The ADLF rose marginally when the GO concentration was raised
3.4.4. Acid durability test to 0.04 % with SSP-20 % (Fig. 19). In both normal and snail shell-based
The findings are provided as “Acid Durability Loss Factor (ADLF), GO-cement composites, the ADLF values were lower at 2 % H2SO4 and
which combines Acid Weight Loss Factor (AMLF), Acid Attacking Factor HCl acidic solutions than at 5 %. Snail shell based GO-cement composite
(AAF), and Acid Strength Loss Factor (ASLF)”. Normal cement com­ specimens outperformed than regular cement composite specimens in
posite specimens suffer greatly in acidic environments owing to acidic situations.
increased capillary voids. Acids may readily penetrate into the com­
posite structure via capillary gaps, causing additional interactions

8
S. Alla and S.S. Asadi
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Fig. 15. Flexural strength of hardened cement composite at GO content 0.01%, 0.02%,0.03% and 0.04% wt. of cement with SSP-20% by the replacement of cement.
TE
AC
R
ET
Fig. 16. Compression strength of hardened cement composite at GO content 0.01%, 0.02%,0.03% and 0.04% wt. of cement with SSP-20% by the replacement
of cement.
R
3.4.5. Microstructure modification of snail shell based GO cement
composite material
Snail shell based graphene oxide cement composite material has
superior mechanical and durability qualities. A scanning electron mi­
croscope (SEM) was used to examine the microstructure of cured cement
composite samples. This is evident in the SEM micrographs of the
hardened mix control specimen (OPC). Fig. 20 (a) shows the hardened
mix micrograph with huge voids and tiny fractures. But the GO and snail
shell powder addition makes the cement composite specimens denser
and more compacted, as demonstrated in Fig. 20 (b), (c), (d) & (e). This
was “due to the snail shell powder’s higher pozzolanic nature and the
inclusion of GO, caused to the formation of hydration crystals such as
Calcium Silicate Hydrate gel (C–S–H), Calcium Hydroxide (Ca(OH)2,
CH), calcium tri-sulfoaluminate (Ca6Al2(SO4)3 (OH)12⋅26H2O) also
known as ettringite (AFt) and calcium mono-sulfoaluminate (AFm) in
the cement composite. Ettringite is also observed in SEM analysis and is
presented as rod-like crystals which are obtained in the early stages of
reaction and are filling pores in cement composite. The hardened
specimens improved binding centers improved the hydraulic
9
Construction and Building Materials 362 (2023) 129767
capabilities of snail shell-based GO-cement composite specimens.
Furthermore, the nucleation of hydration products on nanoparticles
would facilitate the acceleration of cement hydration as well as the
improvement of mechanical and durability properties. The formed
minerals during the hydration are helps to occupy the voids in composite
and formed the denser structure. The formed denser structure is also
responsible for the improvement in durability and mechanical proper­
ties. Based on the findings, it was hypothesized that combining graphene
oxide with snail shell powder can systemize evenly dispersed hydration
products, resulting in a densified and compacted structure in cement
composites.
4. Discussions
This research concentrated for the improvement of fluidity and
workability properties of Graphene Oxide (GO) based cement composite
material. Because, the addition of GO to the cement composite lowered
the fluidity and workability by raising the viscosity. In this case, more
water is needed than the w/c ratio indicates to increase fluidity. The
S. Alla and S.S. Asadi Construction and Building Materials 362 (2023) 129767

D
Fig. 17. % of water absorption of snail shell based GO-cement composite samples.

TE
AC
R
ET

Fig. 18. Water sorptivity coefficient of snail shell-based GO-cement composite samples.
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graphene oxide percentages of 0.01 wt%, 0.02 wt%, 0.03 wt% and 0.04
Table 6
wt% by the weight of cement. We built ordinary cement paste com­
RCPT values of snail shell based GO-cement composite samples in terms charge
posites also to compare the GO and snail shell powder based cement
passed in coulombs.
composites. In addition, microstructure, mechanical and durability
Mix Passage of Charge Permeability of
properties of snail shell-based graphene oxide hardened cement com­
(Coulombs) Chloride Ion (ASTM C
1202) [28]
posite was also determined.
Workability of cement paste has reduced a lot when 0.04 % GO was
GO-0 % 4090 High
added to the mix. In this study, it was found that adding GO to cement
>4000
GO-0.01 % SSP-20 2904 2000–4000 Moderate
% may make the cement paste more viscous. The electrostatic interactions
GO-0.02 % SSP-20 2368 between GO and cement particles produce agglomeration and clumping
% in cement composites. Graphene oxide nanoparticles have a large sur­
GO-0.03 % SSP-20 1872 1000–2000 Low
face area and are hydrophilic, making them less fluid. The addition of
%
GO-0.04 % SSP-20 2048 2000–4000 Moderate snail shell powder enhanced the fluidity of the GO cement composite,
% according to the results. This was mostly owing to the beneficial prop­
erties of snail shell powder, such as its very tiny particle size, low water
demand, and higher pozzolanic nature, which all played a key role.
additional water may reduce the strength. To increase the fluidity of GO- Then, by filling the void spaces in the flocculation structure of GO
cement composites, snail shell powder is used as a substitutive material cement composite with SSP particles, the cement composite may be free
to the cement in the GO based cement composites. In this study, a snail of confinement, resulting in increased fluidity. The preliminary fluidity
shell powder substitute of 10 %, 15 %, and 20 % was studied with of 255 mm was achieved at a maximum 20 % replacement of SSP in GO

10
S. Alla and S.S. Asadi
Fig. 19. Acid durability loss factor of snail shell based GO-Cement composite samples at 28 days.
D
cement composite.
The mechanical and durable properties of snail shell based GO-
cement composite material were increased than the conventional
TE
cement composite specimens at 3, 7, and 28 days of curing. According to
“the gradual increment of GO dosages from 0.01 % to 0.04 % along with
snail shell powder replacement at various percentages to the weight of
the cement, the compression and flexure strength results of GO-Cement
composite samples were increased at 3, 7 and 28 days of curing,
compared to the strength results of normal cement composite mixes”.
AC
Among all mixes, at each GO dosage from 0.01 % to 0.04 % with 20 %
snail shell powder higher strength values was achieved at 3, 7, and 28
days of curing. “After 28 days of curing, the samples with (GO-0.03 %,
SSP-20 %) mix percentage had a 63.47 % increase in flexural strength
compared to the samples without graphene oxide (GO) and SSP”. But at
increased GO dosage (GO-0.04 %, SSP-20 %), the flexure strength of
R
cement composite was reduced, due to the clustering of graphene oxide
nanoparticles at higher dosage of GO addition in cement composite
samples. The compression strength of the cement composite with (GO-
0.04 %, SSP-20 %) mix fraction improved by 42.6 % after 28 days of
ET
curing compared to the samples without GO and SSP.
In the durability aspect, the maximum resistance to water absorption
was recorded at GO-0.03 % and SSP-20 % sample mixes. Conversely, all
snail shell-based GO-cement composite mixes displayed superior water
resistance compared to the traditional sample mixes. In the same
manner, the maximum resistance to water sorptivity was found in the
R
sample mixes with GO-0.03 % and SSP-20 %, but at 0.04 % with SSP-20
%, the resistance to water sorptivity was reduced because GO particles in
the cement composite started to get stuck together. The cement com­
posite samples with SSP-20 % at 0.01 % and 0.02 % GO addition
exhibited moderate chloride permeability; at 0.03 % GO addition
exhibited low chloride permeability; and at increased GO content at
0.04 % exhibited again moderate chloride permeability, due to the
clustering of graphene oxide nanoparticles at higher dosage of GO
addition in cement composite samples. After “28 days immersion in 2 %
and 5 % concentrations of both H2SO4 and HCl acid solutions”, the
highest drop in Acid Durability Loss Factor (ADLF) was recorded for GO-
0.03 % and SSP-20 % sample mixtures. The ADLF rose marginally when
the GO concentration was raised to 0.04 % with SSP-20 %. Based on the
overall findings, it was hypothesized that combining graphene oxide
with snail shell powder can systemize evenly dispersed hydration
products, resulting in a densified and compacted structure in cement
composites.
11
Construction and Building Materials 362 (2023) 129767
5. Conclusions
From the detailed experimental investigation on “Fluidity, Micro­
structure, Mechanical and Durability Properties of Snail Shell based
Graphene Oxide Cement Composite Material” the subsequential con­
clusions are drawn.
1. The addition of snail shell powder enhanced the fluidity of the GO
cement composite, according to the results. This was mostly owing to
the beneficial properties of snail shell powder, such as its very tiny
particle size, low water demand, and higher pozzolanic nature,
which all played a key role.
2. Then, by filling the void spaces in the flocculation structure of GO
cement composite with SSP particles, the cement composite may be
free of confinement, resulting in increased fluidity. The preliminary
fluidity was 255 mm at a maximum 20 % replacement of SSP in GO
cement composite.
3. The mechanical and durable properties of SS based GO-cement
composite material were increased than the conventional cement
composite specimens at 3, 7, and 28 days of curing.
4. When compared to controlled cement composite samples, a 63.47 %
increase in flexural strength was reached at GO-0.03 % and SSP-20 %
sample mixes, and a 42.6 % increase in compressive strength of 0.04
% GO with SSP-20 % was observed after 28 days.
5. With the inclusion of GO as little as 0.03 % with SSP-20 %, the
cement composites durability features such as water absorption and
rapid chloride permeability are reduced by 20–40 %, which is
greater than the cement composites including nano-TiO2 and nano-
SiO2
6. The addition of GO in cement composites improved the resistance to
water sorptivity and acidic environmental impacts significantly.
7. From the micro structural analysis, the densified and compacted
structure in snail shell-based graphene oxide cement composite
samples was observed on SEM images.
CRediT authorship contribution statement
Suseela Alla: Methodology, Formal analysis, Resources, Investiga­
tion, Writing – original draft, Writing – review & editing, Visualization,
Project administration. S.S. Asadi: Methodology, Validation, Visuali­
zation, Supervision, Project administration.
S. Alla and S.S. Asadi Construction and Building Materials 362 (2023) 129767

A B

C-S-H Gel C-S-H Gel

Pore

C D

C-S-H Gel
C-S-H Gel

D
Star ng of E ringite

TE
Void
AC
E

E ngite
R

E ngite
ET
R

Fig. 20. SEM images of cement composites at 28 days mixed with GO and SSP: a) GO-0 % SSP-0 %, b) GO-0.01 % SSP-20 %, c) GO-0.02 % SSP-20 %, d) GO-0.03 %
SSP-20 %, e) GO-0.04 % SSP-20 %.

Declaration of Competing Interest for the smooth conduction of research work”.

The authors declare that they have no known competing financial

interests or personal relationships that could have appeared to influence
the work reported in this paper.
Data availability
The data that has been used is confidential.
Acknowledgements
“The authors are thankful to the CoEAMMPAC for conducting XRD,
SEM, and EDS and thanking the VFSTR for the support and lab facility
Funding
No external funding was used for the research.
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