Journal of Building Engineering 86 (2024) 108963

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Journal of Building Engineering

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

Effect of hemp fibers and crystalline admixtures on the properties

and self-healing efficiency of lime and clay-based mortars
Tsampali Evangelia , Vitta Ioanna , Maria Stefanidou *
Laboratory of Building Materials, School of Civil Engineering, Aristotle University of Thessaloniki, 56124, Greece

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

Keywords: This study investigates the impact of hemp fibers on two fiber-reinforced compositions, clay-
Hemp fibers based and lime-pozzolan mortar. Three compositions were prepared for each mortar, reference
Clay samples without fiber incorporation, samples with untreated hemp fibers, and samples with hy­
Lime-pozzolan drothermally treated hemp fibers with crystallines. Crystalline admixtures (CAs) were incorpo­
Self-healing rated into the hydrothermal pretreatment of fibers to promote the self-healing properties of the
Strength recovery
mortar when needed. Physico-mechanical and thermal properties took place to address the
Crystallines
overall effect of hemp on the mortars. Adding hemp fibers enhanced the mechanical strength and
reduced the mortars’ shrinkage. The hydrothermally treated fibers have better cohesion with
mortars, preserving the best results. To evaluate self-healing efficiency, pre-damaged cubic
samples from each composition were subjected to tap water immersion for lime-pozzolan mortars
and a controlled humid chamber for clay mortars after a curing period. The healing rate was
assessed by measuring crack closure, compressive strength recovery, and the dynamic modulus of
elasticity recovery. The results indicated significant strength recovery in lime-pozzolan mortars
with hemp fibers. Clay-based mortars showed moderate strength increases and limited self-
healing.

1. Introduction
In recent years, integrating natural fibers into traditionally brittle construction materials has emerged as a noteworthy area of
research. This shift is fired by a rise in interest towards eco-friendly and sustainable construction practices, driven by the recognized
benefits of using natural fibers as reinforcements in cement, lime-based, and clay mortars. The appeal of these materials has grown due
to their enhanced mechanical properties, positioning them as desirable choices for sustainable building practices [1–4].
In exploring fiber reinforcement in construction materials, it’s critical to consider natural and synthetic fibers, each offering unique
benefits and drawbacks. Each type of fiber has corresponding advantages that enhance the materials’ properties and limitations.
Natural fibers, such as hemp, flax, jute, and sisal, are environmentally friendly, renewable, and biodegradable, making them highly
appealing for sustainable construction practices. They are known for their good tensile strength, low density, and thermal insulation
properties [5,6]. However, their variability in quality, susceptibility to moisture absorption, and potential degradation over time pose
challenges for consistent performance and durability in construction applications [7,8].
On the other hand, artificial fibers, including glass, steel, and synthetic polymers, provide high strength, durability, and resistance

Abbreviations: HF, hemp fibers; FRM, fiber-reinforced mortars; FRCM, fiber-reinforced clay mortars; FRLPM, fiber-reinforced lime-pozzolan mortars; CAs, crys­
talline admixtures; RCS, recovery of compressive strength.
* Corresponding author.
E-mail address: stefan@civil.auth.gr (M. Stefanidou).

https://doi.org/10.1016/j.jobe.2024.108963
Received 17 November 2023; Received in revised form 8 February 2024; Accepted 28 February 2024
Available online 1 March 2024
2352-7102/© 2024 Elsevier Ltd. All rights reserved.
T. Evangelia et al. Journal of Building Engineering 86 (2024) 108963

to environmental factors. They contribute significantly to the flexural and tensile strength of composite materials. Despite these ad­
vantages, concerns over their environmental impact, energy-intensive production processes, and potential health risks during
manufacturing and disposal highlight the need for careful use [9]. Balancing the benefits and limitations of both fiber types is crucial
for optimizing the performance and sustainability of construction materials, necessitating ongoing research and development in this
area [8,10].
This study added hemp fibers (HF) to lime-pozzolan and clay-based mortar. Hemp fiber, derived from the Cannabis sativa plant, has
a rich history of utilization covering over 10,000 years [11]. As a member of the Cannabis genus, classified under the Rosales order and
the Cannabinaceae family [12], hemp has been a material of choice due to its unique properties. The extraction process involves the
mechanical separation of the bast fibers from the plant. The woody core of the plant, known as hemp shiv, is primarily composed of
cellulose (44%), hemicellulose (18–27%), and lignin (22–28%), among other constituents [6]. The historical significance of hemp is
underscored by archaeological evidence dating back to 8000 BCE [13]. The fiber’s exceptional tensile strength and resistance to
alkalinity have been key factors in its historical use for reinforcement purposes [14]. The application of hemp fiber has expanded to
various sectors including construction, textiles, and bio-based materials.
Using fibers in lime mortars has historical roots, tracing to ancient times. Lime mortars have been widely used in constructing and
restoring historical buildings in places such as India, Italy, Greece, and Egypt [13]. In India, incorporating plant and animal-derived
additives into lime mixtures was a prevalent method to boost their strength, durability, and mechanical characteristics while managing
porosity [15]. However, lime mortars present certain challenges, especially when compared to cement mortars. Notably issues related
to water permeability, which could potentially lead to problems.
Furthermore, the porosity within the lime matrix closely relates to the mortar’s strength and endurance, implying a careful balance
is needed in its composition [16]. The solution to those problems is the incorporation of pozzolans into the mortar matrix, which
significantly impacts the water/binder ratio, bound water, mechanical strength, and pore structure [17]. The evolution of pore
structure occurs in different phases during the setting process, involving dehydration, carbon dioxide penetration, and the formation of
calcium silicate hydrate (C-S-H) and calcium carbonate [17,18]. Given the challenges and opportunities presented by lime-based
materials and hemp-lime mortars, this study proposes developing fiber-reinforced lime-pozzolan mortars (FRLPM). This mortar
composition aims to harness the synergistic benefits of lime and pozzolans while incorporating hemp stems to enhance material
performance, sustainability, and environmental compatibility. Through complete exploration and analysis, this research aims to
explain the promising potential of FRLPM as a resilient and ecological alternative for several construction applications.
Moreover, fiber-reinforced clay-based mortars (FRCM) are well-recognized for their environmentally friendly and natural adhesive
properties, making them desirable components within the sustainable construction sector. However, research examining the physical
properties of FRCM has been limited. Addressing this gap, researchers [19] explored the possibility of clay as a binder for hemp
composites and found that the hemp-to-binder ratio significantly influenced mechanical properties.
This research also focuses on the self-healing potential of FRCM and FRLPM. Self-healing materials have the fundamental ability to
autonomously repair damage induced by stress autonomously, eliminating the need for external intervention. The RILEM Technical
Committee 221-SHC Report [20] has introduced a self-healing terminology framework based on outcomes and processes [21]. These
highlight the distinction between autogenous self-sealing, where the natural components of the material repair crack, and autonomous
self-healing, which, in addition to sealing, also restores the material’s properties. Autonomous self-healing involves altered additives
for crack sealing, while paired with property restoration, it establishes autonomic/engineered self-healing.
Historically, lime-based mortars have shown instances of self-healing, frequently serving as an advantageous feature in ancient
masonry structures [22–24]. However, methodical material design aimed at these properties has been limited. Several studies also
focusing on the self-healing capabilities of lime-based mortars have highlighted the necessity for adapting evaluation methods that
differ significantly from those used for cement-based mortars [25,26]. Lubelli et al. [27] identified self-healing mechanisms in
lime-based mortars involving calcium compound dissolution, transportation, and re-precipitation to mend cracks. A critical
requirement is the ample presence of free lime and moisture. Nardi et al. [20] investigated the effectiveness of crystalline admixtures
and lime/cement-coated granules in the engineered self-healing capacity of lime mortars. The study proved that the presence of
crystalline admixtures in the mortar matrix enhances the aforementioned self-healing capacity due to the delayed hydration and
carbonation of the lime as well as to the reaction of the admixtures with the Ca(OH)2, resulting from the lime hydration.
The self-healing ability of clay mortars represents a fascinating area of study within sustainable building materials, offering a
glimpse into the ancient practices that could inform modern construction. This natural repair mechanism, inherent in clay-based
materials, is attributed to the rehydration of clay particles and the subsequent filling of cracks that may develop over time.
Research by Bobpa et al. [28] shows how clay mortars can autonomously repair minor damages by swelling clay minerals, effectively
sealing cracks, and improving durability. Further, a study by Mahammandi and Choobbasti [29] investigated the effect of the
self-healing process on the increase in strength in clay soil by adding nanomaterials. This study showed the potential for self-healing,
although the self-healing of clay mechanism is not well known. Additionally, self-healing was directly related to the amount of
nano-clay added and the duration of maintenance of samples. These investigations underscore the potential of clay mortars in pre­
serving the structural integrity of buildings and reducing maintenance costs and environmental impact, reaffirming the relevance of
traditional materials in contemporary construction practices.
In this study, the hydrothermal treatment of HF was conducted to enhance self-healing properties employing CAs. Crystalline
Admixtures (CAs) are among the most frequently employed admixtures in the construction sector. Generally commercialized, these
admixtures have proprietary formulas that are not publicly disclosed, making their molecular structure challenging to determine.
Mailvaganam’s classification [30–32] distinguishes CAs as either reactive or inert based on their impact on the hydration process.
Reactive CAs include reactive silicates, finely ground blast-furnace slag, and pozzolans [30]. Inert CAs are commonly represented by

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talc, though bentonite and other siliceous powders are also found. The ACI Committee 212 [33] formally divides CAs into two cat­
egories: Permeability Reducing Admixture for Hydrostatic (PRAH) and Permeability Reducing Admixture for Non-Hydrostatic
(PRAN). This categorization is based on their ability to reduce water permeability under varying pressure conditions. PRAHs are
primarily used as waterproofing agents that reduce the permeability of cementitious materials and facilitate crack healing [26,34,35].
CAs identified as PRAHs have been implemented in concrete mixes to act as permeability-reducing agents that enhance the durability
of concrete structures [31,32,36,37]. Several studies have focused on improving concrete durability by applying CAs, leading to
changes in capillarity, porosity distribution, and interconnectivity within the material [32,38]. Studies investigating the self-healing
properties of lime and clay-based mortars reinforced with HF and crystalline admixtures are rare.
This study investigates the self-healing properties of lime and clay-based mortars reinforced with hemp fibers and crystalline
admixtures. It focuses on evaluating the improvements in mechanical strength, durability, and the ability of these materials to repair
themselves after cracking. By incorporating sustainable hemp fibers and innovative hydrothermal processes with crystalline tech­
nologies, the research aims to enhance the performance and longevity of construction materials, contributing to more durable and
environmentally friendly building practices. The value of this research lies in investigating two environmentally friendly mortars with
lime and clay and the ability of natural fibers to enhance both properties and healing capacity.

2. Materials and methods

2.1. Materials
The raw materials used in this research involved clay, lime, and pozzolan as binders. The clay was bought and processed utilizing a
crusher instrument to ensure proper particle size distribution. Subsequently, the clay particles were sieved through a stainless-steel
double-ring frame with a 500 mm mesh size to attain the desired particle size range. The chemical compounds and the particle size
analysis of raw materials are shown in Table 1. According to that, there is a bid loss of ignition of 15.58% for clay, with the remaining
5% attributed to the error in the measurement and the loss. This percentage is considered normal.
Table 2 indicates the composition of the mortars produced. Accordingly, the lime:pozzolan ratio was always 1:1, and the binder:
aggregate ratio was always 1:2 for all compositions. Besides the clay, lime, and pozzolan, the essential materials required for the study
comprised water (H2O), and a superplasticizer was incorporated to achieve the required workability. Superplasticizer is a new gen­
eration range-reducing admixture based on chains of modified polycarboxylic ether. The sand utilized in the experiments was silicate
sand from 0 to 4 mm. The mixing process followed the standard EN1015-2:1998. The HF used were initially separated and trimmed to
less than 3 cm, then carefully introduced into the mixture to ensure uniform distribution. Specifically, 1.5% of the total mixture volume
was added to incorporate HF into the mix, with a 1.07 g/cm3 density. The water content incorporated into all the compositions was the
same, with a water-to-binder ratio of 0.65 for lime-pozzolan mortars and 0.71 for clay mortars. As for all the compositions, the
workability was maintained at 150 ± 10 mm, as per EN 1015-3:1999. The superplasticizer added to the mixture was adjusted to
preserve the same workability. For each composition 12 prisms (40 × 40 × 160) mm3, 12 cubes (40 × 40 × 40) mm3, 10 cubes (50 ×
50 × 50) mm3, 2 plates (200 × 200 × 30) mm3, and one prism (25 × 25 × 250) mm3 have been prepared. Table 3 provides the details of
the number of specimens, dimensions, and standards for each test.

2.2. Curing conditions

For lime-pozzolan mortars, samples were placed in a controlled environment (65% RH, 22 ± 2 ◦ C) and covered with damp linen to
minimize shrinkage. For clay mortars, samples were placed in the lab environment (60% RH, 22 ± 2 ◦ C) and covered with damp linen
to minimize early shrinkage. Drying shrinkage evaluations followed ASTM C596-14 guidelines and utilized 25 × 25 × 250 mm3
specimens cured at 50% RH and 22 ± 2 ◦ C. Careful specimen handling ensured optimal development of mechanical properties,
including strength and durability.

Table 1
Characterization of raw materials, lime, natural pozzolan, and clay.

Method Lime Natural pozzolan Clay

Density (g/L) ASTM-C188:95 2.279 2.395 2.652

Loss of ignition (%) RT-1000 ◦ C – 5.39 15.58
Cl− % wt. IC <0.01 0.22 <0.01
SO−4 2 % wt. IC 0.29 0.10 0.10
CaO % XRF 87.40 1.37 12.90
MgO% XRF 0.84 0.36 5.22
SO3% XRF 0.49 0.15 0.95
Fe2O3% XRF 0.08 1.34 7.34
AL2O3% XRF 0.03 14.60 12.27
SiO2% XRF – 69.81 37.10
K2O% XRF – 3.02 1.79
Na2O % XRF – 2.87 0.41
TiO2% XRF – 0.36 0.67
MnO% XRF – – 0.11
Particle size (μm) D (0.1) 1.29 1.51 2.69
D (0.5) 3.37 5.11 23.70
D (0.9) 16.04 34.49 215.16

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Table 2
Mix designs of the investigated compositions.

Materials (kg/m3) Compositions

LP LP1 LPcr CL CL1 CLcr

Limestone 302 302 302 – – –
Pozzolan 302 302 302 – – –
Clay – – – 870 870 870
Sand (0–4 mm) 1206 1206 1206 1741 1741 1741
Hemp Fibers (% v/v)a – 1.5 – – 1.5 –
Hydrothermal treated hemp fibers with CAs (% v/v)a – – 1.5 – – 1.5
Superplasticizer (% w/w)b – 1.07 1.07 1.75 4.00 2.00
w/b 0.65 0.65 0.65 0.71 0.71 0.71
Workability (mm) 155 153 155 152 135 155
a
By volume of the mixture.
b
By weight of the binder.

Table 3
Number of specimens, dimensions, and standards for each test.

Shape and Size Number of Specimens/Test Physic/mechanical Property Evaluated Standard Test Methods

Prisms (40 × 40 × 160) mm3 3 Flexural Strength EN 14651:2005

Dynamic Elastic Modulus EN 12504-4:2004
Karsten EN 16302:2013
Cubes (40 × 40 × 40) mm3 3 Compressive Strength EN 196-1:1994
Porosity RILEM CPC 11.3
3
Cubes (50 × 50 × 50) mm 8 Compressive Strength EN 196-1:1994
Dynamic Elastic Modulus (Self-healing tests) EN 12504-4:2004
3
Plates (200 × 200 × 30) mm 1 Thermal conductivity measurement DIN EN 12667:2001
Prisms (25 × 25 × 250) mm3 1 Shrinkage ASTM C596-14

2.3. Physic-mechanical properties

Compressive and flexural strength tests were performed following the EN196-1:1995 standard. Flexural strength tests utilized
specimens measuring 40 × 40 × 160 mm3, while compressive strength tests were carried out on specimens with dimensions of 40 × 40
× 40 mm3. The modulus of elasticity was determined through the Ultrasonic dynamic method, based on EN 12504-4:2004, employing
a specialized instrumentation setup comprising a PROCEQ PUNDIT LAB + UPV INSTRUMENT. Porosity, considered a significant
indicator of open spaces within mortar structures, was measured using the liquid absorption method, as it seemed suitable for small
and irregularly shaped clay mortar samples [39]. This method is based on Archimedes’ principle and involves drying the samples,
removing air, vacuuming, and filling them with n-heptane [40]. The vacuum treatment of the samples followed a modified RILEM CPC
11.3 standard, which accelerated the penetration of the liquid into finer pores [39–41]. For lime-pozzolan mortar compositions, tests
took place after 28, 90, and 180 days of curing. However, for clay specimens, tests were limited to 90 and 180 days due to lacking
early-stage strength. Water penetration assessments were executed through the TQC Karsten Tube Penetration test, according to EN
16302:2013 standard. In this method, a water-filled glass tube was attached to the test material, and vertical water absorption levels
were quantified over time, as specified in Table 4. This test took place after 28 days for lime-based mortars and 90 days for clay
mortars.
Dimensional alterations indicative of material shrinkage were systematically measured in a climate-controlled chamber maintained
at 23 ± 2 ◦ C and a relative humidity of 50 ± 5%. For thermal conductivity (λ) evaluation, plate-shaped specimens with dimensions of
200 × 200 × 30 mm3 were tested using the "Thermtest HFM 100 Series" apparatus, based on EN 12667:2001 standard [42].

2.4. Post-cracking behaviour of the brittleness index of mortars

The goal of adding fibers to mortars is to control crack width, enhancing load-bearing capacity and durability [43]. Flexural
strength was assessed using a universal testing machine with a three-point bend fixture, focused on analyzing load-CMOD curves.
Typically, a notch is engineered into specimens to ensure controlled failure; however, this proved challenging for sensitive,
low-strength mortars based on clay. Therefore, an electronic extensometer was used to quantify crack openings. This data was
f
analyzed to calculate both the proportionality limit strength fct,L and the residual reduced strength fR,j specific CMODj values (j = 1,2,3,
4), according to EN 14651:2005 [44].

Table 4
Intervals over which the KARSTEN test measurement was obtained for each mortar.

KARSTEN Water Absorption Test

Composition LP LP1 LPcr CL CL1 CLcr

Time Distance of each Measurement’s Repetition 5 min 1 min

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T. Evangelia et al. Journal of Building Engineering 86 (2024) 108963

2.5. Processing of hemp fibers

The incorporated fibers in CLcr and LPcr compositions were exposed to treatments of hydrothermal and cryostasis-based chemical
methods to optimize their composite material performance. Initially, the hydrothermal treatment involved steam exposure at 140 ◦ C
and 1.5 atm for 2 h within a specialized reactor. Post-treatment, the fibers were conditioned at 20 ± 2 ◦ C and 65 ± 3% relative hu­
midity. Subsequently, the chemically stabilized fibers were treated with CAs in distilled water, mixed for 10 min, and left for 30 min for
solution penetration. After draining the excess solution, the fibers were air-dried until reaching constant weight under controlled
conditions (20 ± 2 ◦ C, 60 ± 5% relative humidity). The untreated fibers (HF) demonstrated greater stiffness and rigidity in comparison
to their hydrothermally modified counterparts, which were characterized by a "fluffier" texture and reduced stiffness.
To analyze the effects of the treatment on the fibers, both Scanning Electron Microscopy (SEM) and absorption analysis have been
carried out. For Scanning Electron Microscopy, a Jeol JSM-6390LV, Oxford Instruments (Abingdon-on-Thames, UK), was used to
observe the threated and the untreated fibers. Additionally, the water absorption of each type of fiber was measured.

2.6. Evaluation of self-healing

After a curing period of 28 days for the lime-pozzolan mortars and after 90 days for the clay mortars, the specimens were subjected
to controlled pre-damage and pre-cracking tests. Specifically, cubic samples 50 × 50 × 50 mm3 were pre-damaged using a controlled
compressive strength approach. The methodology for the pre-damage test is presented in Table 5. After that, lime-pozzolan mortar
specimens were immersed in tap water maintained at 20 ◦ C ± 2 ◦ C, whereas the clay compositions were placed in a humidification
chamber with conditions set at 80% relative humidity and 40 ◦ C. The humidity is considered necessary for the activation of CAs.
Before each test, the samples were dried in an oven set at 40 ◦ C, until stable weight. The hydration reaction that occurs within the
body of the samples was vital for both healing cracks and improving the overall strength of the material. CAs have hydrophilic
properties, meaning they need water to activate their function. Once water is available, these CAs interact with it, forming a hard
substance that effectively seals the cracks [45,46].
The modulus of elasticity underwent testing following EN 12504-4:2004 standards. Subsequently, the specimens were subjected to
controlled compressive forces until surface cracks measuring 50–300 μm in length became apparent. Following the compression
process, the specimens were re-weighed, and the dynamic modulus of elasticity was recalculated, accounting for the influence of the
newly formed cracks. Initial crack measurements, conducted on day 0, were carried out before subjecting the specimens to healing
conditions. Crack dimensions on the pre-damaged cubic specimens were systematically recorded by optical microscope immediately
after pre-damage and after 14, 28, and 60 days of healing. A portable Dino-Lite microscope was employed for these measurements, and
image analysis was conducted via Dino-Capture 2.0 software to ensure precision and accuracy. An analytic and schematic repre­
sentation of healing conditions and tests is presented in Table 6.
The Crack Closure ratio was calculated according to Equation (1):
CWinitial(t0 ) − CWhealed(Δt)
Crackclosure = ∗ 100 (%) (1)
CWinitial(t0 )

Where:
Crackclosure = Crack closure ratio (%)
CWinitial (t0) = Crack width after pre-crack, (μm).
CWhealed (Δt) = Crack width after t days of healing (μm).
Additionally, eight cubic specimens 50 × 50 × 50 mm3 for each composition were pre-damaged at 28 days for the lime-pozzolan
mortars and at 90 days for the clay mortars, up to 80 % of the initial corresponding compressive strength. Afterward, these specimens
underwent a healing period of 180 days under distinct conditions and were then re-tested until failure. The recovery of compressive
strength (RCS) was quantified using Eq. (2):

Table 5
Pre-damage test, for all prismatic specimens.

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Table 6
Schematic representation of healing conditions and tests for its evaluation.

Composition Healing Condition Pre-cracked and Recovery of Dynamic Recovery of Crack Closure Number of
pre-damaged at Modulus of Elasticity (RDM) compressive Specimens
strength (RCS)

Measured after

Lime-Pozzolan W Immersed in tap 28 days (0 days of healing) 180 days of healing 14, 28, and 8
mortars water at 20 ◦ C 28 days of curing, before and 60 days of
±2 ◦ C after pre-cracking/damage and healing
Clay mortars HC Humidity 90 days 60, and 180 of healing
Chamber
95% Rh and 40 ◦ C

Phealed(t=180days)
RCS = ∗ 100 (%) (2)
Punhealed

Where:
RCS = Rate of recovery of compressive strength (%)
Phealed (t = 180 days) = Compressive strength after healing (t = 180 days), (MPa).
Punhealed = Initial compressive strength (MPa).

3. Results and discussion

3.1. Physic-mechanical properties
Fig. 1 depicts the compressive strength of the lime-pozzolan mortars and clay mortars. In both types of mortar, it was found that the
incorporation of fibers increased the compressive strength across all the curing ages. Furthermore, the compositions containing hy­
drothermally processed fibers exhibited superior performance. Specifically, after 180 days of curing, the compressive strengths of LP1
and LPcr increased by 4% and 62%, respectively, compared to the reference sample. For clay mortars, the strengths of CL1 and CLcr
were determined to be 28% and 35%, respectively, greater than the reference sample at the same curing duration of 180 days.

3.1.1. Dynamic modulus of elasticity

Fig. 2 presents the results of the dynamic modulus of elasticity for lime-pozzolan and clay mortars. Analyzing the results at 28 days,
the lime-pozzolan reference mortar (LP) displayed a higher modulus than the fiber-reinforced mortar (FRM). This observation can be
attributed to the presence of fibers contributing to the increase of pores within the LP mortars, probably due to the poor adhesion of
fibers to the matrix. On the contrary, the lime-pozzolan composition LPcr displayed the highest dynamic modulus of elasticity at 180
days, at 14.0 GPa, similar to the reference, showing the beneficial effect of crystallines in the mixture, with composition CLcr exhibiting
the highest dynamic modulus of elasticity at 180 days, at 14.0 GPa.
The dynamic modulus of elasticity for the clay mortars aligned with the compressive strength results, showing improved properties
for the fiber-modified composition. The CL and CLcr had the greatest dynamic modulus of elasticity, with CLcr presenting slightly
better results. The percentage increase in dynamic modulus from 90 to 180 days was 1.35%, 3.8%, and 0.5% for CL, CL1, and CLcr,
respectively.

Fig. 1. Compressive strength of the (a) lime-pozzolan mortars at 28, 90, and 180 days, and (b) clay mortar at 90 and 180 days of curing.

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Fig. 2. Dynamic modulus of elasticity of (a) lime-pozzolan mortars at 28, 90, and 180 days, and (b) clay mortar at 90 and 180 days of curing.

3.1.2. Flexural strength

The flexural strength diagrams of the lime-pozzolan and clay mortars are depicted in Fig. 3. For the LP compositions, it was visible
that the highest flexural strength was reached by the LPcr mortars, while the reference composition exhibited the lowest flexural
strength. Particularly, the flexural strength of LP1 and LPcr after 90 days was 10% and 34%, respectively, greater than the reference.
Similarly, within the clay mortar compositions, a notable increase in flexural strength was observed for the CLcr mortars, which is
followed closely by the mortars reinforced with untreated HF, CL1. As was expected, the reference mortar composition, CL, displayed
the lowest flexural strength, as HF are well known to be compatible with clay. For clay mortars, an increase of approximately 24% was
noted for the mortars incorporating the untreated fibers, while the mortars with the hydrothermal processed fibers exhibited an in­
crease of around 43% after 180 days of curing.

3.1.3. Relation of compressive and flexural strength

Fig. 4(a) illustrates the correlation between flexural and compressive strength across all lime mortar samples at 28, 90, and 180
days. The analysis reveals a modest correlation, with an R2 value of 0.4604. This limited correlation is attributed to factors such as
cohesion, the integration of fibers within the matrix, and their contribution to the overall strength. Conversely, Fig. 4(b) explores the
same relationship for clay mortars at 90 and 180 days, uncovering a solid correlation, evidenced by an R2 value of 0.911. This indicates
a robust cohesion and uniform distribution of hemp fibers within the clay mortar, highlighting the effectiveness of fiber reinforcement
in enhancing the material’s mechanical properties.

3.2. Evaluation of the brittleness index of mortars

From the data presented in Figs. 4 and 5, the notable influence of fibers in clay and lime-based mortars was determined. The
remaining strengths, FR,j, were calculated for the respective CMODj values (j = 1, 2, 3, 4). F1 concerned to CMOD = 0.5 mm, F2 to
CMOD = 1.5 mm, F3 to CMOD = 2.5 mm, and F4 to CMOD = 3.5 mm. Essentially, for specific deformations, the corresponding loads
were evaluated. Afterward, using Eq.(4), the remainder strength of each composition was calculated, represented as the mean of the

Fig. 3. Flexural strength of the (a) lime-pozzolan mortar compositions at 28, 90, and 180 days, and (b) clay mortar at 90 and 180 days of curing.

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T. Evangelia et al. Journal of Building Engineering 86 (2024) 108963

Fig. 4. Compressive and flexural strength relationship for (a) Lime mortars after 28, 90, and 180 days and (b) Clay mortars after 90 and 180 days.

Fig. 5. CMODj and the corresponding values of fR,j for (a) lime-pozzolan mortar and (b) clay mortar after 90 days of curing.

distinct deformations. For the lime-based mortars, as depicted in Figs. 5(a) and 6(a), the superior performance was demonstrated by
LPcr. It was observed that the hydrothermally modified HF treated with crystallines accelerated the adhesion with the mortar matrix.
This acted as a crack-bridging agent, mitigated the mortar’s granular texture, and impeded crack progression. It was logically
concluded that compositions without fibers would exhibit non-ideal results, given the absence of fibers to mitigate stresses and foster a
more regulated failure process. About the clay mortars, as illustrated in Figs. 5(b) and Fig. 6(b), the most effective synergy between HF
and the matrix was exhibited by the CL1 composition. The FR,j values exhibited considerable uniformity with gradual reduction for 90
days. The minimum strength value, as expected for the stipulated CMOD, was, predictably, observed in the compositions without

Fig. 6. ffct,L for (a) lime-pozzolan mortar, and (b) clay mortars after 90 days of curing.

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hemp.

3.2.1. Porosity
In Fig. 7, the porosity of lime-pozzolan and clay mortars is illustrated. Upon comparing the compressive strength with the porosity
of the three lime-pozzolan mortars at 28 days, the LP1 and LPcr compositions exhibited the highest porosity. However, the two
compositions had different behaviors toward strength. It’s speculated that stiffer fibers, when integrated into the mortar matrix,
succeeded in stronger cohesion with the matrix and increased the mechanical properties. Notably, the porosity of LPcr was lower than
that of LP1. In the case of LPcr, the results underlined that the hydrothermally modified fibers decreased the porosity over time and
enhanced the compressive strength for all tested ages. Except for the porosity alteration, the mortars’ specific gravity has changed,
according to Table 7. The fibers’ incorporation decreased the mortars’ specific gravity, further explaining the greater porosity.
In contrast, the inclusion of HF in the clay mortar matrix resulted in reduced porosity. This reduction was greater with the addition
of the hydrothermally processed fibers at 90 and 180 days of curing. The porosity of CL1 and Clcr has been reduced by 13% and 23%,
respectively, after 180 days of curing, compared to CL mortars. The relationship between compressive strength and porosity is in
complete agreement in this context; as porosity decreases, strength increases. In contradiction with the porosity results, the specific
gravity of the clay mortars has reduced by over 20%. However, this can be attributed mainly to the low specific gravity of the HF.
The decrease in porosity with the increase in fibre content, contrary to expectations from the literature, could be due to the fibres
enhancing the density and structural integrity of the mortar. Hemp fibers might fill voids within the mortar matrix, reducing overall
porosity. Additionally, the fibers promote a more uniform distribution of particles and a tighter packing structure; this could also lower
porosity. This phenomenon suggests that the specific interaction between HF and the mortar matrix, possibly including fiber-matrix
bonding and the physical blocking of voids by fibres, plays a crucial role in altering expected outcomes regarding porosity.

3.2.2. KARSTEN water absorption test

In the Karsten test (Fig. 8), it was observed that the lime-pozzolan mortars with hydrothermally modified HF and crystallines (LPcr)
exhibited the most pronounced water absorption. Conversely, the reference mortar devoid of fibers was found to have the lowest water
absorption. Given that water absorption is directly correlated with porosity, the test outcomes seemed to be deemed consistent, as they
were tested at 28 days of curing. Nevertheless, the Karsten test was performed on the surface of the specimens representing the
exposure to rain. The role of the fibers is limited in this test. Additionally, their hydrophilic nature could explain the recorded values in
Fig. 8.
For the clay mortars, the tests were performed after 90 days of curing, and the highest water absorption rate was found in the
mortar containing untreated fibers. The absorbency was noted to be greater than that of the reference compositions. The composition
with treated HF and added CAs was determined to have the best performance, displaying the highest resistance to water absorption.
Based on all the sample measurements, it was noted that the largest continuous volume of water was absorbed at the beginning of each
test and during the initial minutes. The rate stabilized to a level notably lower than the initial rate.
According to the results, samples containing clay have higher water absorption rates than those with lime due to clay’s inherently
more porous structure and fine-grained texture, enhancing capillary absorption and enabling greater water uptake. This characteristic,
combined with the hydrophilic nature of HF used, further increases the moisture-holding capacity of clay-based mortars. These factors
collectively contribute to the observed higher water absorption rates in clay samples compared to their lime samples.

3.2.3. Shrinkage
Shrinkage has been identified as a primary contributor to crack initiation, accelerating the deterioration of materials [47]. The
mechanism investigated in this paper was the drying shrinkage, which is induced by the loss of moisture after the curing of the material
(Fig. 9). Integrating fibers as reinforcement in lime-based mortar has been identified as one of the most effective methods to enhance
tensile strength while limiting plastic shrinkage. The synergy between lime, clay, and HF resulted in effective collaboration. The

Fig. 7. Porosity (%) for the (a) lime-pozzolan mortars at 28, 90, and 180 days, and (b) clay mortars at 90 and 180 days of curing.

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Table 7
Porosity (%) and Specific gravity (g/cm3) on the curing day of the Karten test.

LP LP1 LPcr CL CL1 CLcr

28 days 90 days
Porosity (%) 27.50 32.50 30.15 16.92 16.28 13.76
Specific gravity (g/cm3) 1.87 1.73 1.74 2.65 2.03 1.85

Fig. 8. Average water absorption (ml) per minute for all the mortars, 28 days of curing for lime-based mortars, and 90 days for clay mortars.

Fig. 9. Length shrinkage to time’s square root in (a) lime-based mortar compositions and (b) clay mortars.

produced mortars were characterized by appropriate workability, with no indications of segregation or inconsistency. Within the
studied compositions, the greater shrinkage was exhibited by LP and CL, whereas CLcr and LPcr revealed the less dimensional
reduction. It should be highlighted that the highest water loss was observed across all compositions during the initial weeks of
observation, predominantly due to coagulation and solidification mechanisms. After that, a plateau in the measurements was reached.
The increased drying contraction observed in LP and CL is believed to have arisen due to the lack of fibers. However, similar results for
CL and Cl1 may be due to the plain HF being moistureless. On the other hand, the hydrothermally modified LPcr and CLcr fibers’
slightly hydrated state resulted in minimum shrinkage.

3.2.4. Thermal conductivity measurement

Stagnant air has a low coefficient of thermal conductivity and is, therefore, a poor conductor of heat. Its very small mass (due to its
low density) makes it extremely difficult to transfer heat. The thermal conductivity coefficient λ of a porous material is lower than the λ
of the same material if it were more compact. Fig. 10 depicts the thermal conductivity and thermal resistance results at 10 ◦ C and 20 ◦ C
for all the mortars, 28 days of curing for lime-pozzolan mortars, and 90 days for clay mortars. By starting with the lime-based mortars,
the fibers acted positively regarding thermal conductivity since the compositions containing fibers (LP1, LPcr) have reduced λ and

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Fig. 10. Thermal conductivity results at 10 ◦ C and 20 ◦ C for all the mortars, 28 days of curing for lime-based mortars, and 90 days for clay mortars.

almost the same between them, both at 10 ◦ C and 20 ◦ C. As mentioned above, fibers increase porosity and consequently offer a lower
conductivity coefficient due to trapped air. At the opposite end of the spectrum are the clay mortars in which the reference composition
showed the best thermal insulation capacity. In contrast, the fiber compositions acquired a more compact structure with less trapped
air during setting in accordance with the porosity measurements. It is worth mentioning that clay-based mortars presented lower λ
values in comparison to the lime-pozzolan in all tested scenarios.

3.3. Evaluation of self-healing

In Fig. 11(a) and (b), the dynamic modulus of elasticity for the mortars is depicted at various healing stages: at 28 days of curing,
before and after the pre-damage, and following 60 and 180 days of healing. It was observed that the dynamic modulus of elasticity for
the cubic lime-based mortars significantly increased upon immersion in tap water. The most pronounced increase in dynamic elastic
modulus was recorded at 60 days. The composition demonstrates that the greater increase was for LPcr mortar. In contrast, the clay
compositions did not surpass the properties of their original structure, as indicated by the dynamic modulus of elasticity values at 60
and 180 days of healing, which did not exceed the 90-day curing pre-cracking value. Nevertheless, the healing conditions were found
to dense the mass structure of the specimens and the pore distribution, as reflected by the stabilization of the elastic modulus after 60
days of healing at a value markedly higher than that immediately post-cracking.
Cubic specimens measuring 50 × 50 × 50 mm3 were pre-damaged at 80% of their initial compressive strength, measured at 28 days
for lime-pozzolan compositions and at 90 days for clay compositions. This initial strength was determined as the average from three
individual specimens. The recovery of compressive strength (RCS) after a 180-day healing period is illustrated in Fig. 12 and computed
by Eq. (2).
It was noted that compositions incorporating untreated HF exhibited superior recovery results. The RCS was lower than that of the
reference sample for hydrothermally treated hemp. Specifically, RCS values were 244%, 411%, and 173% for LP, LP1, and LPcr,
respectively. Conversely, the lime-pozzolan mortars demonstrated remarkable recovery capabilities. This recovery can be attributed to
the inherent characteristics of lime, which can dissolve in water and relocate to fill voids in the structural matrix in accordance with the
Ed measurements, as well as to the fiber’s ability to bridge and stabilize cracks. In contrast, the RCS for clay mortars was 76%, 78%,
and 67% for CLY, CLY1, and CLYcr, respectively. Notably, the RCS for all clay mortar compositions was consistently below 100%,
indicating an inability to recover the initial strength.
The crack width of the pre-cracked samples was evaluated using a Dino-Lite microscope to evaluate self-healing, according to Eq.
(1). As presented in Table 8, the initial crack healing process was the development of white precipitates at the crack mouth of the
specimens. The crack width of the lime-based mortars lacking fiber addition decreased markedly, by approximately half compared to
the initial measurement, and after that, exhibited minimal variation until the final 28-day, Fig. 13. For the LP1 composition containing
untreated HF, full closure (100%) of the cracks was achieved by day fourteen, a phenomenon potentially attributable to the fiber
presence, which serves to bridge the crack edges. Hemp, similar to all plants, absorbs atmospheric carbon dioxide (CO2), amplifying
lime’s carbonation and the development process as the lime converts back to limestone [48]. Conversely, in the LPcr mortar, inte­
grating hydrothermally modified fibers with crystallines did not enhance crack healing. This composition’s crack healing rate was
largely analogous to that of the lime reference composition (LP).
In the clay mortars, a significantly lower rate of healing in crack width was observed, according to Fig. 14. At the same time, neither
the incorporation of fibers nor the addition of crystalline admixtures (CAs) proved effective in enhancing the healing process by
harnessing environmental humidity, as the crack width largely remained constant over time.

3.3.1. Treatment effect

The integration of HF into mortar systems has emerged as a promising path for enhancing self-healing capabilities. Notably,

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T. Evangelia et al. Journal of Building Engineering 86 (2024) 108963

Fig. 11. Dynamic modulus of elasticity at 28 days before the samples were pre-cracked, at 28 days right after they were pre-cracked, at 60, and 180 days of healing for
(a) lime-pozzolan mortars, and (b) clay mortars.

Fig. 12. Recovery of compressive strength after 180 days of healing occurred in (a) lime-based mortars and (b) clay mortars.

untreated HF outperformed their hydrothermally treated counterparts in self-healing tests. Chemically, untreated fibers likely preserve
a greater amount of native cellulose structures, which are inherently hydrophilic, aiding in moisture absorption crucial for self-healing
through calcium carbonate precipitation. The hydrothermal treatment, while beneficial for amplifying cellulose convertibility, might
compromise the fibers’ intrinsic hydrophilic nature. It could also alter the topography and chemistry of the fiber surface, potentially
affecting its interaction with the calcium-rich healing agents in the mortar matrix. The heat and pressure of the treatment might further
close off micro-pores essential for moisture retention. These observations underscore the delicate balance between fibers’ physical and
chemical modifications and their self-healing efficacy, highlighting the importance of tailored treatments for specific mortar appli­
cations. Fig. 15 illustrates noticeable differences between the untreated and the hydrothermally modified fibers.
Also, a microstructural investigation took place, and representative SEM (Scanning Electron Microscopy) images and EDS analysis,
demonstrating these differences in surface characteristics, are provided in Fig. 16. Subfigures 16(a) and 16(b) showed the untreated
fibers exhibiting rough and pure surfaces. On the other hand, subfigures 16(c) and 16(d) exhibited the hydrothermally treated fibers at
two magnifications, showcasing surfaces modified with attached crystalline admixtures spanning their entire length. Notably, in
specific areas, the CAs appear to agglomerate.
This analysis highlighted the noticeable surface morphological alterations between the untreated and the hydrothermally modified
fibers, emphasizing the impactful surface transformations and crystalline attachments resulting from hydrothermal treatment. An EDS
analysis of the treated surface also established that the crystalline was attached to the surface (Fig. 16(e)). Specifically, the main
compounds of the crystalline were SiO2 and Na2O, with the elements of Si and Na covering the fiber’s surface.
Additionally, an absorption test took place further to understand the effects of the treatments on the fibers. This involved weighing
the dry fibers, immersing them for 24 h, and weighing them again to determine the extent of saturation. In the case of the untreated
fibers, it was detected that they absorbed water equivalent to 4.5 times their weight. Conversely, the treated fibers displayed a reduced
absorption capacity, absorbing water amounting to 3.8 times their weight. This test confirmed that the treatment not only affected the
surface of the fibers but also the physical properties of them.

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Table 8
Microscopic images of the evolution of crack widths at 0, 14, 28, and 60 days of healing, measured with a Dino-Lite microscope.

Fig. 13. Maximum, minimum, and average crack width at 0, 14, 28, and 60 days of healing for (a) LP, (b) LP1, and (c) LCpl mortar compositions.

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Fig. 14. Maximum, minimum, and average crack width at 0, 14, 28, and 60 days of healing for (a) CL, (b) CL1, and (c) CLcr mortar compositions.

Fig. 15. Clay mortars after the flexural test.

4. Conclusions
The research thoroughly explores the impact of treated with CAs and untreated hemp fibers on lime and clay-based mortars’
properties and self-healing efficiency, offering significant insights into sustainable construction materials.
Integrating both untreated and hydrothermally treated hemp fibers significantly improved the mechanical strengths of lime-
pozzolan and clay-based mortars. This enhancement is chiefly due to the fibers’ capacity for effective stress distribution and their
functionality in crack bridging, which reinforces the mortar matrix. The underlying cellulose structure in hemp fibers plays a crucial
role in this reinforcement, where its natural properties contribute to the mortars’ improved tensile strength and durability.
The research highlights the pronounced self-healing potential of lime-pozzolan mortars embedded with hemp fibers, particularly
those untreated. The mechanism for self-healing, driven by the natural process of CO2 absorption and moisture, leads to remarkable
strength recovery and crack closure. However, clay-based mortars exhibit moderate strength enhancements and limited self-healing
abilities. It is inferred that the cellulose content in hemp fibers aids in self-healing by facilitating the precipitation of healing com­
pounds within the cracks.
Applying hydrothermal treatment to hemp fibers and crystalline admixtures demonstrates diverse effects. Although this treatment
advances mechanical properties and reduces porosity, it does not significantly boost self-healing efficiency compared to untreated
fibers. The alteration of cellulose structure through hydrothermal treatment is notable, as it modifies the fibers’ hydrophilic properties
and potentially affects the interaction between the fibers and the mortar matrix. This alteration could contribute to the observed
discrepancy in self-healing efficiency, indicating the complexity of cellulose’s role in the material’s performance.
In conclusion, the study underscores the promising contribution of hemp fibers to improving mortars’ structural and self-healing
properties, with a particular focus on the crucial role of cellulose alteration through treatments. These findings underscore the
importance of further research to unravel the intricate relationship between cellulose structures in natural fibers and their efficacy in
construction applications, aiming to advance sustainable and resilient building materials.

CRediT authorship contribution statement

Tsampali Evangelia: Writing – original draft, Investigation, Data curation. Vitta Ioanna: Software, Data curation. Maria Ste­
fanidou: Writing – review & editing, Supervision, Methodology, Conceptualization.

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T. Evangelia et al. Journal of Building Engineering 86 (2024) 108963

Fig. 16. Images of SEM analysis for untreated (a) & (b), treated fibers (c) &(d), and EDS analysis of the surface of the treated hemp fiber.

Declaration of competing interest

In relation to the submitted original research paper entitled “Investigating the self-healing properties of lime and clay-based
mortars reinforced with hemp fibers and crystalline admixtures” by Tsampali Evangelia, Vitta Ioanna and M. Stefanidou for
possible publication in Journal of Building Engineering the authors would like to declare that there is no actual or potential conflict of
interest including personal or other relationships with other people or organizations that could inappropriately influence the present
work (Declarations of competing interests: none).

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Data availability

Data will be made available on request.

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