International Journal of Heat and Mass Transfer 130 (2019) 431–439

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International Journal of Heat and Mass Transfer

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

Experimental and numerical investigations on the effect of alkaline

hornification on the hydrothermal ageing of Agave natural fiber
composites
Deepak Jain a,b,⇑, Ishita Kamboj a, Tarun Kumar Bera a, Amardeep Singh Kang c, Rohit Kumar Singla a
a
Mechanical Engineering Department, Thapar Institute of Engineering & Technology, Patiala 147004, India
b
Department of Biomedical Engineering and Mechanics, Virginia Polytechnic Institute and State University, Blacksburg, VA 24061, USA
c
I. K. Gujral Punjab Technical University, Kapurthala 144603, India

a r t i c l e i n f o a b s t r a c t

Article history: Experimental and numerical investigations are performed to evaluate the mass diffusion in Agave
Received 1 August 2018 Americana natural fiber composites considering several environmental conditions. The effect of fiber
Received in revised form 23 October 2018 pretreatment by alkaline hornification is analyzed on the moisture uptake behavior of the Agave fiber
Accepted 25 October 2018
composites. It was observed that water retention value, which is a measure of affinity towards moisture,
Available online 30 October 2018
reduces with each subsequent hornification cycle. The microstructural investigations were performed to
analyze the morphological changes in fiber microfibrils. Composite specimens were subjected to acceler-
Keywords:
ated ageing under water and humidity conditions at controlled temperatures between 0 °C and 75 °C.
Mass diffusion
Natural fibers
Composites were weighted periodically and mass gain curves were analyzed. A comparison is drawn
Fiber pretreatment between the mass gain behavior of composites fabricated using untreated and alkali hornified Agave
Microstructural investigations fibers. The studies have revealed a clear influence of alkaline hornification on the improvement of the
Fick’s law hydrothermal durability of the Agave fibers. The effective moisture diffusivity of the composites is deter-
Finite element analysis mined using edge correction factors for rectanguloid specimens. Finally, the experimental mass gain is
compared with the numerical Fick’s law based finite element (FE) approximations.
Ó 2018 Elsevier Ltd. All rights reserved.

1. Introduction as lignin, hemicellulose, wax, and other water soluble components

With a promising range of mechanical and physical properties
natural fibers have become potential alternative materials. An
increase in research activities in this direction is driven by several
promising features of these fibers such as reasonable mechanical
strength, biodegradability, and low cost of these fibers in compar-
ison to synthetic fibers. Amidst several benefits, a key barrier in the
extensive deployment of natural fibers is their affinity towards the
moisture and water in the service environments. The prolonged
exposure in thermal and moisture service environments may
result in matrix plasticization, swelling, hydrolysis, oxidation,
interfacial de-cohesion between fiber and matrix [1–3].
Several fiber pre-treatment methods have been proposed in the
past to reduce the moisture susceptibility of these fibers. Pretreat-
ment of the fibers with different alkali concentrations improved
the surface roughness and removal of non-cellulosic content such
⇑ Corresponding author. Address: Room No. CD-105, Mechanical Engineering
Department, Thapar Institute of Engineering & Technology, Patiala 147004, India
E-mail address: deepak.jain@thapar.edu (D. Jain).
reduced the water uptake in several types of natural fibers [4–6].
The removal of the impurities and improved surface roughness
also enhanced the elastic modulus of several natural fibers [7–9].
As an alternative approach, the fiber pretreatment by cyclic horni-
fication can also reduce the water retention inside many naturally
available fibers [10–12]. Chemical treatment of Agave fibers with
maleic and acetic anhydride reduced the water uptake and
improved the fiber matrix bonding [13]. Besides, alkali treatment
resulted in an improved fiber-matrix adhesion, tensile and com-
pressive strength of the Agave fibers [14].
The authors observe that there doesn’t exist any literature on
the assessment of alkaline hornification on the properties of Agave
fibers. Further, there is no literature available which consider the
combined effect of temperature and humidity on the Agave fiber
reinforced composites. The objective of the present work is to
determine the combined effect of water, humidity and tempera-
ture on both untreated and alkali hornified fiber composites. The
microstructural investigations were conducted to reveal the
morphology after subsequent hornification cycles. Water retention
values were evaluated at the end of each hornification cycle. We

https://doi.org/10.1016/j.ijheatmasstransfer.2018.10.106
0017-9310/Ó 2018 Elsevier Ltd. All rights reserved.
432 D. Jain et al. / International Journal of Heat and Mass Transfer 130 (2019) 431–439
consider the temperatures in a range of 0–75 °C with both humid-
ity and water exposure conditions. The analytical investigations
were done to deduce the effective diffusivity from the respective
mass gain curves under different conditions. Toward the end, we
perform Fick’s law based finite element analysis (FEA) and com-
pare the numerical and the experimental results.
2. Experiment details
2.1. Materials
The Agave Americana fibers were used as the reinforcements.
They were off-white to yellow in color with a semi-dull appear-
ance. The fiber length was
2.8 m and fiber diameter was 100–
150 mm. The substantial presence of cellulose and hemicellulose
content is a key reason for the high moisture susceptibility of these
fibers in comparison to other natural fibers. Table 1 represents the
density, moisture and typical material constituents of Agave Amer-
icana fibers.
The commercially available epoxy resin LY556 and hardener
HY951 (Huntsman) were used as matrix materials. The extra pure
sodium hydroxide pellets (Sigma Aldrich) were used for the cyclic
alkali hornification.
2.2. Alkaline hornification
Fiber hornification can be considered as an accelerated ageing
of the natural fibers under controlled conditions to improve their
microstructural properties. The swelling of cellulose during the
soaking cycle increases its dimensional stability. In addition, the
formation of an irreversible hydrogen bond with the repetition of
the hornification cycles reduces the water retake inside the inter-
fibrillar space [11]. In the soaking cycles, the alkali treatment is
known to remove lignin, wax, and other water soluble compounds.
In the alkaline hornification, the fibers were soaked in a water bath
with 8% (w/v) alkali concentration. In the present fiber pretreat-
ment process, the temperature and time duration for the
subsequent soaking and drying cycles were followed after experi-
mental conditions [11,17–18]. Fig. 1 shows the experimental setup
for alkali hornification of fibers. During the soaking cycles, the
fibers were immersed in a water bath for 2 h under a temperature
of 23 °C. Each soaking cycle was followed by drying of the fibers
Table 1
Constituents of Agave Americana fibers [15, 16].
Density Moisture Cellulose Hemicellulose Lignin
1.36 g/cm3 7–9% 68–80% 15% 5–17%
Fig. 1. Cyclic Hornification (a) Soaking in the water bath and (b) Drying in the furnace.
inside the furnace maintained at 110 °C for four hours. The temper-
ature was reduced gradually at the end of the drying cycle to avoid
the thermal shocks. Therefore, after 4 h of continuous drying at
110 °C, the temperature was reduced gradually by 5–10 °C after
every 5 to 10 min in the last one hour. The alternate soaking and
drying together form one cycle. Four such cycles were conducted.
The visual and hand evaluation of the hornified fibers revealed
changes in surface texture, shape, and color of these fibers. Fig. 2
(a–e) shows the fiber textures at the end of successive drying
cycles. The change in color is evident from the off-white color of
unconditioned fibers to bumblebee color of conditioned fibers.
Although the natural fibers do not possess a fixed diameter, the
shrinkage of the hornified fiber was apparent when compared with
the untreated fibers.
Water retention value (WRV) is a standardized method to calcu-
late the amount of water retained in the fibers after successive
soaking cycles. It is commonly used as a measure for the quantita-
tive assessment of the natural fiber’s affinity towards the moisture.
It is expressed according to Eq. (1) as [11]:
ðM w  M d Þ
WRV ¼ ð1Þ
Md
Here, Mw and Md are wet and dry mass measured after subse-
quent Soaking and drying cycles. Table 2 shows the WRV at differ-
ent stages of hornification.
Fig. 3 shows a gradual reduction in water retention capacities of
Agave fibers at the end of each hornification cycle. The percentile
hornification measures the overall drop in WRV. The fibers condi-
tioned after the 4th cycle was used in the preparation of the com-
posite specimen for moisture diffusion experiments.
2.3. Microstructural investigations
The microstructural fiber morphology was studied through
scanning electron microscopy (SEM). The fiber cross sections were
analyzed for both untreated and alkali hornified fibers after each
hornification cycle. SEM micrographs were recorded on JEOL
(6510LV) series scanning electron microscope. The test samples
were gold coated to avoid electrical charge accumulation. Fig. 4
shows the SEM images of the fiber cross-section at two different
resolution scales of 100 and 20 mm. The untreated fiber cross sec-
tions in Fig. 4(a) shows a possible presence of non-cellulose amor-
phous components such as wax, lignin and hemicellulose within
the microfibrils. The partial removal of these components and
other water soluble residues after the first hornification cycle
and shrinkage of the fiber cells at the end of second hornification
Wax cycle is noticeable. The regions enclosed inside dashed yellow rect-
0.26%
angles show a shrinkage of fiber cells due to soaking followed by
drying in subsequent hornification cycles. The shrinkage around
 D. Jain et al. / International Journal of Heat and Mass Transfer 130 (2019) 431–439 433

(a) Untreated (b) Cycle-I (c) Cycle-II (d) Cycle-III (e) Cycle-IV

Fig. 2. The texture of (a) Untreated, and alkali hornified fibers after (b) cycle I (c) cycle II, (d) cycle III, and (e) cycle IV.

were Length (l) = 76.2 mm, Width (w) = 24.5 mm, and Thickness
Table 2
WRV and% hornification. (h) = 3 mm. These dimensions were taken according to ASTM
D570-98 [19] standard test method for moisture diffusion.
WRV for each cycle of hornification (%)
The specimens were placed inside a forced air circulation
0 cycle 1 cycle 2 cycles 3 cycles 4 cycles % hornification humidity chamber with the temperature control constancy of
200 176.1 158.6 149.1 145.3 27.4 ±1.0 °C. At a relative humidity of 70% the specimens placed under
three different temperatures conditions of 25 °C, 50 °C & 75 °C. In
the water absorption experiments, we chose four different temper-
atures viz. 0 °C, 25 °C, 50 °C & 75 °C. A cryostat water bath capable
220 to maintain sub-zero temperatures was used for maintaining 0 °C
temperature condition inside water. A digital water bath was used
for the other three temperature conditions of 25 °C, 50 °C & 75 °C.
200 The specimens were weighed on an electronic analytical balance
having a readability of 0.1 mg. The mass gain was measured peri-
odically. Before weighing, the specimens were removed securely
and it was ensured that they are wiped dry to get rid of any undue
WRV (%)

180
160
140
0 1 2 3
Hornification cycle Number
Fig. 3. WRV with the number of hornification cycles.
the voids results from the collapse of fiber cell walls and formation
of microcracks after 2nd, 3rd and 4th cycle of hornification. These
cracks are visible in relatively higher resolution images in Fig. 4
(c2), (d2) and (e2). The crack formation is mainly because of the
excessive fatigue of fiber cell walls due to soaking and drying.
2.4. Specimen fabrication and hydrothermal ageing
Thermosetting matrix was prepared by mixing resin (LY556)
and hardener (HY 951) according to the industrial specifications
in a ratio of 10:1. The composite sheets were fabricated using hand
lay-up method followed by compression loading and curing under
room temperature. The sheets were cured at the room temperature
for 7 days. The composite sheets were finally machined into the
rectanguloid strip shape specimens. The dimensions of specimens
surface moisture. The mass gain is measured according to the Eq.
(2):
Wt  WO
Mt ¼  100% ð2Þ
WO
Here, M t is the instantaneous percentile mass gain, W t is the
measured weight, and W O is the initial weight of the specimen.
Fig. 5 shows the mass gain profiles under the different environ-
ments. Throughout the graphs, we use a nomenclature ‘X-YZ’ to
4
define an environmental condition. Here X designates the type of
fiber treatment. X as ‘UN’ means untreated, whereas ‘AH’ means
alkali hornification. Y indicates exposure to water (W) or humid-
ity(H) condition and Z indicates the temperature condition. As an
example, AH-H50 refers to the composite specimen fabricated
using alkali hornified (AH) fibers, subjected to humidity (H) condi-
tion at 50 °C.
Fig. 5(a) plots the mass gain for the composites subjected to
humidity and temperature inside the moisture chamber. The
specimens were placed inside the moisture chamber for approx-
imately 400 h. A sharp rise in mass gain can be noticed initially
due to the high concentration gradient between the exterior
environment and a composite specimen with the dry interior.
The moisture diffuses mainly through the gaps within the poly-
mer chains of epoxy matrix. The sharp rise is followed by a
decline in the rate of mass gain. Most of the specimens attained
the moisture saturation within 350 h. After this, they didn’t
show any considerable mass gain. The fiber pretreatment
showed a high influence on the moisture uptake throughout
the exposure duration. Under the similar environmental condi-
434 D. Jain et al. / International Journal of Heat and Mass Transfer 130 (2019) 431–439

Untreated (a1) (a2)

Fibers

After
(b1) (b2)
Cycle I

After
(c1) (c2)
Cycle II Microcrack

Lume

After
(d1) (d2)
Cycle III
Microcrack

After (e1) (e2)

Cycle IV

Microcrack

Fig. 4. SEM micrographs of the fiber cross-section at different pretreatment stages.

tions, with a lower mass gain, alkali hornified fiber specimens
has a lower mass gain in comparison to the untreated Agave
fiber specimens. The moisture sorption experiments clearly
quantify the effect of fiber modification on the improvement in
the hydrophobicity of alkali horrified fiber specimens. The natu-
ral fibers have a complex composite structure which influences
the moisture diffusion mechanism. Presently, there is a limited
knowledge of molecular processes and chemical kinetics on
moisture diffusion. However, it is well known that during the
moisture sorption, the crystalline and closely packed hydrophilic
cellulose structures allows the moisture to penetrate though the
less oriented amorphous regions consisting of non-fibrous pec-
tins, hemicellulose and lignin. These amorphous regions are
highly susceptible to moisture as water/moisture can penetrate
further through these regions only [20]. During the alkali horni-
fication, the reaction with hydroxyl groups in the fibers leads to
the removal of moisture susceptible hemicellulose and lignin
compounds. It can be explained as:
Fiber-OH þ NaOH ! Fiber-O Naþ þ H2 O
 D. Jain et al. / International Journal of Heat and Mass Transfer 130 (2019) 431–439 435

UN-H75 Untreated fibers / Water exposure

1.4 (a) Humidity Chamber 7
Alkali Hornified fibers / Water exposure
UN-H50 Untreated fibers / 70% RH
1.2 6 Alkali Hornified fibers / 70% RH

1.0 AH-H75 5

Mass Gain (%)

Mass Gain (%)

0.8 AH-H50 4

0.6 3
UN-H25
0.4 2
AH-H25
0.2
1

0.0
0 100 200 300 400 0
0 25 50 75
Time (Hr.) Temperature (oC)

Fig. 6. Comparison of mass gain at different environmental conditions.

7 (b) Water Bath UN-W75

6
of fiber cell walls which results in reduced moisture permeability
[10,11]. Similar observations can be made in Fig. 5(b) and (c) plots
AH-W75
Mass Gain (%)

5 for the exposure to the water at different temperatures. The mass

UN-W50 gain was much lower in pre-conditioned fiber specimens. The
4 effect of elevated temperatures on the diffusion behavior is also
AH-W50 evident. The rate of mass gain (initial slope of the curves) and final
3 UN-W25 mass gain increased with the increase in temperature. This is
because of the increased diffusivity at higher temperatures. Fig. 6
2 AH-W25 compares the mass gain measured at the end of 14 days. It was
the time when most of the specimens reached a saturation stage.
1 In comparison to untreated fiber composites, the alkali hornified
composites showed an average mass gain about 45%, 24%, 21%
0 and 28% lower at 0 °C, 25 °C, 50 °C & 75 °C respectively. Similarly,
0 50 100 150 200 250 300 350 under the humidity conditions the mass gain was about 30%,
Time (Hr.) 27%, and 26% lower at 25 °C, 50 °C & 75 °C.

3.0 3. Numerical investigations

(c) Cryo Bath UN-W0
2.5 The mass gain curves for most of the specimens showed a sig-
nificant moisture uptake initially for several days which is followed
by the pseudo saturation plateau. Such a behavior can reasonably
Mass Gain (%)

2.0 be considered as a Fickian diffusion [22,23]. As a part of numerical

investigations, first, we first evaluate the moisture diffusion
AH-W0 coefficient of different composite specimens from their respective
1.5
mass gain curves. The calculated diffusion coefficients were used
in subsequent Fick’s law based finite element procedure to find
1.0 the theoretical mass gain.

3.1. Evaluation of moisture diffusion coefficients

0.5
To find the moisture diffusion coefficient ðDc Þ of monolithic
0.0 composite specimen, we ignore the topological effects of fiber dis-
0 100 200 300 400 500 tribution and assume it as homogeneous and isotropic. Therefore,
Time (Hr.) it is reasonable to assume that diffusion coefficients ðDx ; Dy ; Dz Þ
are same in all the three directions (X, Y, and Z) along with a rect-
Fig. 5. Mass gain vs. time plots for environmental exposure inside (a) Environ- anguloid model that represents a composite specimen. Fig. 7 shows
mental chamber at 70% R.H (b) Water bath at 25 °C, 50 °C & 75 °C, and (c) Cryostat
the model geometry similar to experimental specimens. When a
bath at 0 °C.
specimen is immersed in water/humidity conditions, the three-
dimensional moisture uptake is assumed to follow Fick’s law of
diffusion:
The increase in crystallinity due to removal of these cementing !
amorphous compounds leads to a better packing of cellulose chain @c @2C @2C @2C
and improves the fiber matrix adhesion of the composite [21]. Also, ¼ Dc þ þ ð3Þ
@t @x2 @y2 @z2
the subsequent hornification cycles results in irreversible closure
436 D. Jain et al. / International Journal of Heat and Mass Transfer 130 (2019) 431–439

UN-W50
1.0
X

0.8

0.6

Mt/Mα
Y

Z 0.4

0.2
h

Fig. 7. Specimen geometry and rectangular coordinates. 0.0

0.00 0.05 0.10 0.15 0.20 0.25
[Time(Sec.)]1/2 / Length
The solution of Eq. (3) upon volume integration is used to calcu- pffiffiffiffiffiffiffiffiffiffi
Fig. 8. Mt =M1 vs time/length plot of UN-W50 specimen.
late the fractional mass uptake as [24]:
 3 X 1 X 1 X 1
rffiffiffiffiffiffiffiffi
Mt 8 1 Mt 4 Dx t
¼1  ¼ ð8Þ
M1 P2
p¼0 q¼0 r¼0 ðð2p þ 1Þð2q þ 1Þð2r þ 1ÞÞ
2
M1 l p
h   2   2   i
p2 tDeff 2pþ1 Using the edge correction factor for the 3-dimensional mass dif-
2
þ 2qþ1 þ 2rþ1
e l w h
ð4Þ fusion, Eq. (8) is rewritten as:
rffiffiffiffiffiffiffi
where M t is instantaneous mass and M1 is saturation mass. Eq. (4) Mt 4f Dc t
¼ ð9Þ
also states that a saturation state exists when fractional mass M1 l p
uptake asymptotes to unity.
Rearrangement of Eq. (9) gives the slope of the initial portion of
The rectanguloid specimens used in experiments have thickness
the mass gain curve as:
h
3 mm. It is much smaller than the other two dimensions (l, w).
rffiffiffiffiffiffi
For the approximation of Dc , we use the procedure stated for the Mt =M 1 Dc
S ¼ pffiffi ¼ 4f ð10Þ
thin rectanguloid shapes [25] under an initial assumption that
t =l p
the moisture uptake in the composite occurs only along the
broader face parallel to XY plane. To compensate for the edge and finally, Eq. (10) can be rearranged as:
effects, an edge correction factor (f ) is suggested as:  2
sffiffiffiffiffiffi sffiffiffiffiffiffi sffiffiffiffiffiffiffiffiffiffiffi
p S
Dc ¼ ð11Þ
h Dx h Dy h
2
Dx Dy 16 f
f ¼ 1 þ 0:54 þ 0:54 þ 0:33 ; Dx – Dy – Dz
l Dz w Dz lw Dz In this manner, the respective mass gain curves of different
ð5Þ specimens were analyzed to evaluate their respective moisture dif-
fusion coefficients. Table 3 shows the coefficient of moisture diffu-
For a simplistic estimation of the diffusivity ðDc Þ of monolithic sion for different specimens calculated using Eq. (11).
specimens under the assumptions that:
3.2. Finite element analysis (FEA)
(i) The geometrical effects of the unidirectional fiber arrange-
ment are minimal,
Evaluation of mass diffusion coefficients is followed by the
(ii) and the diffusion coefficient in the composites is the same in
finite element analysis. Fick’s law based commercial finite element
all directions, as it is in the resin. i.e. Dx ¼ Dy ¼ Dz ¼ Dc , the
code Abaqus [26] is used to model the mass diffusion inside the
edge correction factor becomes:
specimen models. To reduce the computational effort, we use the
2
symmetry of the rectanguloid specimens along all the three princi-
h h h pal directions (X, Y, and Z) and model the moisture diffusion in
f ¼ 1 þ 0:54 þ 0:54 þ 0:33 ð6Þ
l w lw 1/8th of the entire volume. Fig. 9 shows the full body model with
pffiffiffiffiffiffiffiffiffiffi the 1/8th meshed region. Assuming a state of constant diffusivity,
Fig. 8 plot the fractional mass gain vs. time=length for one of
the specimen. The diffusion coefficient of the composite is calcu- the Fick’s law is used to find the concentration C(Xi ; t) as the solu-
lated from the slope (S) of this graph. The initial mass uptake yields tion variable inside the modeled volume verified by the boundary
pffiffiffiffiffiffiffiffiffiffi conditions:
a linear increase with time /length. The slope is determined for
the initial portion of the mass uptake curve when M t =M 1 6 0:5. @c
¼ Dc r2 C with CðXi ; tÞ ¼ 0 at t
Under an assumption of one-dimensional mass flow, Eq. (4) @t
reduces to: ¼ 0 in the whole domain Xm ; and ð12Þ

Mt 8 X
1
1 2pþ1 2
e p tDx ð l Þ
2
¼1 2 ð7Þ C ¼ C amb on boundary Cc ð13Þ
M1 P p¼0 ð2p þ 1Þ
2

Here r2 is the Laplacian operator and Cc represents all the three

For M t =M 1 6 0:5, Eq. (7) can be approximated as: boundary surfaces which are exposed to the ambient moisture
 D. Jain et al. / International Journal of Heat and Mass Transfer 130 (2019) 431–439 437

Table 3
Coefficient of moisture diffusion of different specimens.

Type The coefficient of Moisture diffusion (m2/sec)

Humidity Chamber Water Bath
25 °C 50 °C 75 °C 0 °C 25 °C 50 °C 75 °C
Untreated 0.78  1012 1.08  1012 1.12  1012 3.62  1012 4.02  1012 5.56  1012 7.66  1012
Alkali Hornified 0.62  1012 0.96  1012 1.02  1012 1.55  1012 3.86  1012 4.22  1012 5.92  1012

Fig. 9. Moisture diffusion model and FE mesh.

Z
ðC amb Þ. The other three planar surfaces of modeled volume which
MðXm ; tÞ ¼ cðx; y; z; tÞdV ð14Þ
are opposite to moisture exposed surfaces have no mass flux either Xm
entering or leaving through them for the entire duration. Under
Fig. 11(a, b) show the theoretical mass gain of different speci-
these boundary conditions, the moisture ingresses towards the
mens. With the time, a steep initial mass gain is followed by an
dry interior regions. Fig. 10 shows the moisture concentration pro-
asymptotic mass gain that indicates the saturation stage. However,
files for AH-W75 specimen model at different time instances. The
due to the time-bound nature of the experiments and a slower rate
geometry shown in Fig. 10 is the flipped image of the meshed
of mass gain, the mass saturation couldn’t be attained under
region shown in Fig. 9 with the left, bottom and front surfaces as
humidity conditions. It is obvious that the mass gain is according
moisture exposed boundaries and top surface reveals the moisture
to the computed diffusivities. The objective of present analytical
evolution along the specimen interior.
investigations is to determine the theoretical diffusivities and com-
The mass gain, MðXm ; tÞ; by the specimen due to moisture
pare the mass gains determined through FEA approximations with
ingression at time t can be calculated through the volume integral
experimental mass gains. Fig. 12 compares the experimental and
of the moisture concentration at that time. That is,
numerical results for one of the specimens.

75 hr.
10 hr. 40 hr.

bottom
90 hr. 150 hr.

Fig. 10. Moisture concentration profiles inside the 1/8th model.

438 D. Jain et al. / International Journal of Heat and Mass Transfer 130 (2019) 431–439

8 later stages of diffusion. Such deviations can be attributed to resin

(a) Water Exposure deterioration or morphological changes. It is understandable that
7 UN-W75 the effect of such conditions is difficult to predict using the simpli-
fied numerical procedures under the straightforward assumptions.
6 Nevertheless, a close proximity was found between experimental
and FEA predictions for most of the specimens. It also proves that
Mass Gain (%)

5 the stated procedure results in a reasonable prediction of numeri-

AH-W75
UN-W50 cal diffusivities.
4
AH-W50

3 UN-W25 4. Conclusions
AH-W25
UN-W0
2 A comprehensive experimental and numerical study has been
AH-W0 conducted to evaluate the moisture diffusion behavior of Agave
1 fiber reinforced polymer composites. The effect of fiber pretreat-
ment by alkaline hornification is evaluated on the moisture dura-
0 bility assessment in accelerated hydrothermal ageing conditions.
0 100 200 300 400 500
The experimental work was followed by an assessment of moisture
Time (Hr.)
diffusion coefficients of different specimens and finite element
1.4 analysis. The important conclusions drawn from this study are:
(b) Humidity Conditions
UN-H75 1. Fiber pretreatment by alkaline hornification resulted in a signif-
1.2
icant reduction of mass gain of natural fiber composites at all
UN-H50 the temperature conditions under both humid and wet
1.0
environments.
Mass Gain (%)

2. Several irreversible changes in fiber morphology were observed.

0.8 AH-H75
SEM investigations revealed the reduction in lumen size and
AH-H50 partial removal of alkali soluble lignin and water soluble con-
0.6 tents of the fibers with subsequent soaking and drying cycles.
3. The change in microstructural morphology resulted in the
0.4 UN-H25 reduced water retention in agave fibers. A drop in water reten-
tion value by 27% after four cycles of hornification lead to a
0.2 AH-H25 remarkable reduction in mass gain of composites at all the
exposure conditions. The coefficient of moisture diffusion for
0.0 alkali treated Agave fiber specimens reduced by 130% in com-
0 100 200 300 400 500 parison to the untreated specimens at 0 °C.
Time (Hr.) 4. The mass diffusion appears to follow Fick’s diffusion behavior
inside both conditioned and unconditioned composite
Fig. 11. Mass gain vs time under (a) Water exposure (b) Humidity conditions. specimens. The effective diffusivities were derived using edge
correction factor and implementing Fick’s law for the inverse
calculation. The derived diffusivities resulted in a fair prediction
of mass gain through FEA investigations.
1.4 AH-W0 (Experimental)
AH-W0 (Fickian FEA)
The present investigations clearly uncover the underlying
1.2
potential of alkaline hornification for the improvement of moisture
durability of Agave fibers. The effect of similar treatment on the
1.0
Mass Gain (%)

behavior of these fibers in synergistic mechanical and hydrother-

mal ageing environments is still unknown and it is a work in
0.8 progress.

0.6
Conflict of Interest Statement
0.4
The authors declared that there is no conflict of interest.
0.2
Appendix A. Supplementary material
0.0
0 100 200 300 400 Supplementary data associated with this article can be found, in
Time (Hr.) the online version, at https://doi.org/10.1016/j.ijheatmasstransfer.
2018.10.106.
Fig. 12. Experimental vs Analytical results for AH-W0 specimen.

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